Synthesis, molecular structures, and properties of heterometallic cobalt tetramethylcyclobutadiene complexes (C4Me4)Co(CO) 2TePh, (C4Me4)Co(CO)2TePh[W(CO) 5], and Me4C4Co(μ3-S) 2Cr2Cp2(μ-SC4H9)

Article abstract of DOI:10.1007/s11172-007-0268-9

The reaction of Cb*Co(CO)₂I (1) (Cb*is tetramethylcyclobutadiene) with sodium phenyltelluride afforded the mononuclesar complex Cb*Co(CO)₂TePh (2). The reaction of the latter with W(CO)₅(THF) produced the Cb*Co(CO)₂TePh[W(CO) ₅] compound (4). The reaction of 1 with the Cp₂Cr ₂(SCMe₃)₂S complex gave the heterometallic cluster Cb*Co(μ₃-S)₂Cr₂Cp2 (μ-SCMe₃) (5). Complexes 2, 4, and 5 are diamagnetic. Their structures were determined by X-ray diffraction. Complex 2 contains the Co-Te bond (2.585(1) A); complex 4, the Co-Te (2.558(8) A) and W-Te (2.8467(6) A) bonds. Complex 5 has the stable triangular sulfide-and tert-butylmercaptide-bridged core Cr₂Co (Cr-Cr and Cr-Co bond lengths are 2.626(2) and 2.673(2) A, respectively) with Cp ligands at the chromium atoms and a Cb*ligand at the cobalt atom. Complex 5 was characterized by cyclic voltammetry. The thermolysis of complex 4 was studied.

Full text of DOI:10.1007/s11172-007-0268-9

Russian Chemical Bulletin, International Edition, Vol. 56, No. 9, pp. 1731—1735, September, 2007
1731
Synthesis, molecular structures, and properties of heterometallic
cobalt tetramethylcyclobutadiene complexes
(C4Me4)Co(CO)2TePh, (C4Me4)Co(CO)2TePh[W(CO)5],
and Me4C4Co(µ3ꢀS)2Cr2Cp2(µꢀSC4H9)*
a
a
a
a
A. A. Pasynskii,a I. V. Skabitskii, S. S. Shapovalov, A. R. Galustyan, Yu. V. Torubaev,
ꢀ
Zh. V. Dobrokhotova,a V. A. Grinberg,b E. V. Mutseneck,c and A. R. Kudinovc
aN. S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences,
31 Leninsky prosp., 119991 Moscow, Russian Federation.
Fax: +7 (495) 954 1279. Eꢀmail: aapas@rambler.ru
bA. N. Frumkin Institute of Physical Chemistry and Electrochemistry, Russian Academy of Sciences,
31 Leninsky prosp., 119991 Moscow, Russian Federation.
cA. N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences,
28 ul. Vavilova, 119991 Moscow, Russian Federation
The reaction of Cb*Co(CO)2I (1) (Cb* is tetramethylcyclobutadiene) with sodium
phenyltelluride afforded the mononuclear complex Cb*Co(CO)2TePh (2). The reaction of the
latter with W(CO)5(THF) produced the Cb*Co(CO)2TePh[W(CO)5] compound (4). The
reaction of 1 with the Cp2Cr2(SCMe3)2S complex gave the heterometallic cluster Cb*Co(µ ꢀ
3
S)2Cr2Cp2 (µꢀSCMe3) (5). Complexes 2, 4, and 5 are diamagnetic. Their structures were
determined by Xꢀray diffraction. Complex 2 contains the Co—Te bond (2.585(1) Å); comꢀ
plex 4, the Co—Te (2.558(8) Å) and W—Te (2.8467(6) Å) bonds. Complex 5 has the stable
triangular sulfideꢀ and tertꢀbutylmercaptideꢀbridged core Cr2Co (Cr—Cr and Cr—Co bond
lengths are 2.626(2) and 2.673(2) Å, respectively) with Cp ligands at the chromium atoms and
a Cb* ligand at the cobalt atom. Complex 5 was characterized by cyclic voltammetry. The
thermolysis of complex 4 was studied.
Key words: heterometallic complexes, Xꢀray diffraction study, cyclopentadienyl complexes,
cyclobutadiene complexes, metal carbonyls, metal chalcogenides, tungsten, cobalt, chromium,
electrochemistry, thermolysis.
The extensive chemistry of chalcogenide complexes
containing the stable CpFe fragment and its perꢀ
methylated analog has attracted attention in view of the
problem of modeling of natural FeSꢀcontaining enzymes.
In particular, the chalcogenꢀcontaining complexes
CpFe(CO)2XPh (X = S or Se) (Fe—S, 2.282 Å; Fe—Se,
2.413 Å; Fe—S—C, 113.46°; Fe—Se—C, 105.82°)1,2 and
the heterometallic compound CpFe(CO)2SPhW(CO)5
(Fe—S, 2.301 Å; S—W, 2.577 Å; Fe—S—W, 106.44°)3
were reported. In addition, the heterometallic antiferroꢀ
magnetic cluster CpFe(µ3ꢀS)2Cr2Cp2(µꢀSBut) containꢀ
ing the stable Cr2Fe core surrounded by sulfur atoms was
described.4 It was of interest to synthesize analogs conꢀ
taining another metal of life, viz., cobalt, by replacing the
CpFe fragment in these complexes with the isolobal stable
Cb*Co fragment (Cb* is tetramethylcyclobutadiene). The
wide use of the latter fragꢀ
ment was covered in the reꢀ
view.5 The only cobalt comꢀ
plex (A) containing chalcoꢀ
genide and the fourꢀmemꢀ
bered σ,πꢀbonded ring deꢀ
rived from tetratrifluoroꢀ
methylcyclobutadiene has
been structurally characterized.6
Results and Discussion
We used the tetramethylcyclobutadiene dicarbonyl ioꢀ
dide complex Cb*Co(CO)2I (1) (see Ref. 7) as the key
compound for the synthesis of heterometallic chalcoꢀ
genide complexes.
The treatment of complex 1 with sodium phenylꢀ
telluride afforded the mononuclear dicarbonyl complex
Cb*Co(CO)2TePh (2) as redꢀblack crystals characterized
* Dedicated to Academician G. A. Abakumov on the occasion
of his 70th birthday.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1669—1673, September, 2007.
1066ꢀ5285/07/5609ꢀ1731 © 2007 Springer Science+Business Media, Inc.

1732
Russ.Chem.Bull., Int.Ed., Vol. 56, No. 9, September, 2007
Pasynskii et al.
Scheme 1
Table 1. Selected bond lengths (d) and bond angles (ω) in comꢀ
pounds 2* and 4
2
4
Bond
Co(1)—Te(1)
Te(1)—C(11)
d/Å
2.5848(11)
2.113(7)
Bond
d/Å
Co(1)—Te(1)
Te(1)—C(16)
W(1)—Te(1)
2.5578(8)
2.132(4)
2.8469(6)
Angle
ω/deg
Angle
ω/deg
C(11)ꢀTe(1)ꢀCo(1) 98.15(16) C(16)ꢀTe(1)ꢀW(1) 99.94(10)
Co(1)ꢀTe(1)ꢀW(1) 111.899(15)
* For compound 2, the bond lengths and bond angles are given
for one of the two independent molecules, whose geometric
parameters are virtually identical.
In turn, the reaction of complex
2
with
W(CO)5(THF) produces the heterometallic compound
Cb*Co(CO)2TePh•W(CO)5 (4) (Scheme 1). Complex 4
is stable in air, does not undergo decarbonylation under
UV irradiation for 2 h, and crystallizes from diethyl ether,
toluene, or dichloromethane as orange crystals. Accordꢀ
ing to the Xꢀray diffraction study, complex 4 contains
the Co—Te—W group with the Co—Te and W—Te
single bonds (2.558(8) and 2.8467(6) Å, respectively; see
Table 1).
by two CO stretching bands in the IR spectrum (νCO
=
1970 and 1900 cm–1). According to the Xꢀray diffraction
study, complex 1 contains the Co—Te single bond
(2.585(1) Å) (Scheme 1, Fig. 1, Table 1). In addition, we
obtained the product of its
partial decarbonylation as a
black finely crystalline comꢀ
pound characterized by the
only CO stretching band in
In addition, the reaction of
1
with the
the IR spectrum (νCO
=
Cp2Cr2(SC4H9)2S complex9 involves the complete
decarbonylation and elimination of one tertꢀbutyl group
to give the heterometallic cluster Cb*Co(µ3ꢀS)2Cr2(µꢀ
SBut)Cp2 (5) (Scheme 2).
1960 cm–1). According to
the elemental analysis data, this product has structure 3
analogous to many known complexes of this type, for
example, to the [(πꢀC7H7)Mo(CO)(µꢀTePh)]2 complex
described in our earlier publication.8
The Xꢀray diffraction study showed that compound 5
contains the stable triangular core Cr2Co (Cr—Cr,
2.630(2) Å; Cr—Co, 2.674(2) Å) (Table 2) suppleꢀ
mented with µ3ꢀsulfide bridges and cyclopentadiꢀ
enyl and tertꢀbutylthiolate ligands at the chromium
C(8)
C(4)
C(7)
C(3)
C(9)
C(10)
C(6)
C(7)
C(5)
Co(1)
C(6)
O(5)
O(6)
C(5)
C(10)
C(3)
C(2)
C(9)
C(13)
O(2)
C(14)
O(7)
C(15)
Te(1)
C(4)
Co(1)
C(8)
O(2)
C(2)
W(1)
C(1)
Te(1)
C(1)
C(12)
C(11)
O(3)
C(11)
C(16)
O(1)
O(4)
O(1)
C(16)
C(17)
C(21)
C(20)
C(19)
C(12)
C(15)
C(13)
C(18)
C(14)
Fig. 1. Molecular structure of complex 2.
Fig. 2. Molecular structure of complex 4.

Mixedꢀmetal cyclobutadienecobalt complexes
Russ.Chem.Bull., Int.Ed., Vol. 56, No. 9, September, 2007 1733
Scheme 2
C(9)
S(11)
Cr(1´)
Cr(2´)
S(10)
S(15)
Co(2)
C(59)
C(14)
C(27)
C(4)
Fig. 3. Molecular structure of complex 5.
Table 2. Selected bond lengths (d) and bond angles (ω) in comꢀ
pound 5*
ing carbonyl groups had a reversible oneꢀelectron oxidaꢀ
tion wave at –0.11 V (along with an irreversible twoꢀ
electron oxidation wave at +1.09 V). The sandwich comꢀ
plex CpCoCb*, in which the dichromium disulfide fragꢀ
ment of cluster 5 is formally replaced by the isoelectronic
Cp ligand, is characterized by a reversible oneꢀelectron
oxidation wave at +0.26 V and two irreversible oneꢀelecꢀ
tron oxidation waves at +0.66 and +0.99 V, i.e., the
Cp fragment is more electronꢀwithdrawing with respect
to the Cb*Co group than the cluster ligand [Cp2Cr2(µꢀ
SC4H9)(µ3ꢀS)2].
A study of the thermolysis of heterometallic complex 4
under argon showed that the Cb* ligand, like the cycloꢀ
pentadienyl ligand, is eliminated in the last step and that
carbides and oxides are absent among the pyrolysis prodꢀ
ucts, in spite of the fact that the formation of these comꢀ
pounds is typical12 of the thermolysis of carbonylchalcoꢀ
genides at M : X > 1.
Bond
d/Å
Angle
ω/deg
Co(1)—S(2)
Co(1)—S(1)
Co(1)—Cr(2)
Co(1)—Cr(1)
Cr(1)—S(1)
Cr(1)—S(2)
Cr(1)—S(3)
Cr(1)—Cr(2)
Cr(2)— S(1)
Cr(2)—S(2)
Cr(2)—S(3)
2.150(2) Cr(2)—Co(1)—Cr(1) 58.82(5)
2.173(2) Co(1)—S(2)—Cr(2) 73.75(8)
2.674(2) Co(1)—S(2)—Cr(1) 73.88(8)
2.681(2) Cr(2)—S(2)—Cr(1) 69.62(8)
2.264(3) C(19)—S(3)—Cr(2) 116.1(3)
2.306(3) C(19)—S(3)—Cr(1) 116.2(4)
2.363(3) Cr(2)—S(3)—Cr(1) 67.88(8)
2.630(2)
2.280(3)
2.301(3)
2.347(3)
* The bond lengths and bond angles are given for one of the
three independent molecules, whose geometric parameters are
virtually identical.
atoms and a tetramethylcyclobutadiene ligand at the coꢀ
ꢀ
balt atom.
Unlike
the
antiferromagnetic
complexes
Cp2Cr2(SC4H9)2S (see Ref. 9) and Cp2Cr2(µꢀSCMe3)(µꢀ
S)2Co(CO)2 (see Ref. 11) studied earlier, complex 5 is
diamagnetic, which can be due to the electronꢀdonating
properties of the Cb* ligand. Actually, the cyclic
voltammogram of Cp2Cr2(µꢀSCMe3)(µꢀS)2Co(CO)2
showed an irreversible oneꢀelectron oxidation wave at
+0.39 V, whereas the cyclic voltammogram of complex 5
containing Cb* ligands instead of two electronꢀwithdrawꢀ
ꢀ
The presence of three structurally similar independent molꢀ
ecules is associated with a pseudosymmetry, which is not a unique
feature of this structure (see Ref. 10).

1734
Russ.Chem.Bull., Int.Ed., Vol. 56, No. 9, September, 2007
Pasynskii et al.
The elemental analysis was performed on a Carlo Erba
CHNS analyzer.
The IR spectra were recorded on a Specord 75 IR spectroꢀ
photometer in KBr pellets.
The loss of the first two carbonyl groups is accompaꢀ
nied by the endothermic effect. A further rise of the temꢀ
perature leads to the loss of the other CO groups, the
process being highly exothermic. Then the Ph group is
eliminated with a weak endothermic effect, and only the
final exothermic step of thermolysis leads to the eliminaꢀ
tion of the Cb* ring. Presumably, the exothermic proꢀ
cesses of the ligand removal is accompanied by the forꢀ
mation of new M—Te and M—M bonds.
Therefore, the Cb*Co fragment not only forms stable
bonds with chalcogens but also can form heterometallic
chalcogenides by binding other metal atoms through the
chalcogen atom (for example, by binding tungsten through
tellurium) or by supplementing this binding with direct
metal—metal bonds, as in the case of the addition of
sulfur and chromium atoms of the cluster fragment
[Cp2Cr2(µꢀSC4H9)(µ3ꢀS)2].
Xꢀray diffraction study. The crystallographic data and the
Xꢀray diffraction data collection and refinement statistics for
compounds 2, 4, and 5 are given in Table 3. The structures were
solved by direct methods and refined by the fullꢀmatrix leastꢀ
squares method with anisotropic and isotropic thermal paramꢀ
eters (H atoms were refined using a riding model). Semiempirical
absorption corrections were applied based on equivalent reflecꢀ
tions (SADABS). All calculations were carried out with the use
of the SHELXTL program package.13 The principal geometric
parameters for compounds 2, 4, and 5 are given in Tables 1
and 2. The complete tables of the atomic coordinates, bond
lengths, bond angles, and anisotropic displacement parameters
were deposited with the Cambridge Structural Database.
Cyclic voltammograms (CV) of the complexes were reꢀ
corded on a PAR 273 (Princeton Applied Research) potentioꢀ
stat/galvanostat using the standard software. The measurements
were carried out in a temperatureꢀcontrolled threeꢀelectrode
electrochemical cell under specialꢀpurity argon. A SUꢀ2000 disk
glassyꢀcarbon electrode (0.0058 cm2) pressed into Teflon was
used as the working electrode, and a platinum plate with a
surface area of 1 cm2 served as the auxiliary electrode. The
potentials were measured relative to the silver reference electrode
in the same solution and are given relative to the Fc/Fc+ pair.
Experimental
All operations associated with the synthesis and isolation of
the complexes were carried out under pure argon and in anꢀ
hydrous solvents. The Cb*Co(CO)2I (see Ref. 7) and Cp2Cr2(µꢀ
SC4H9)2(µꢀS) (see Ref. 9) complexes were synthesized accordꢀ
ing to procedures described earlier.
Table 3. Crystallographic data for complexes 2, 4, and 5
Parameter
2
4
5
Molecular formula
Molecular weight
C16H17CoO2Te
427.83
C21H17CoO7TeW
751.73
C22H31CoCr2S3
554.58
Diffractometer
T/K
Space group
a/Å
b/Å
c/Å
Bruker Smart CCD
120
Bruker Smart CCD
120
Bruker Smart CCD
120(2)
P–1
P2(1)/n
9.796(2)
16.717(4)
14.852(4)
90
105.434(8)
90
2344.4(10)
4
P2(1)/n
14.207(3)
34.661(7)
15.144(3)
90
112.546(7
90
6887(3)
12
8.3940(17)
13.634(3)
15.634(3)
95.57(3)
104.55(3)
97.68(3)
1700.3(6)
4
α/deg
β/deg
γ/deg
V/Å3
Z
F(000)
ρ
832
1.671
1408
2.130
3432
1.604
calc/g m–3
Radiation, λ(MoꢀKα)/Å
Linear absorption, µ/mm–1
Scanning mode
0.71073
2.689
0.71073
6.867
0.71073
1.923
ω
ω
ω
Scan range/deg
1.52—26.97
2.48—29.00
1.17—26.00
Number of measured reflections
Number of independent reflections
Rint
8019
7399
0.0214
13140
6020
0.0238
48156
13509
0.1094
Number of reflections with [I > 2σ(I )]
Number of parameters
R1
4951
369
0.0521
5478
281
0.0284
7351
757
0.0764
wR2
0.1445
0.0628
0.1535
GOOF
ρ
0.963
1.575/–1.280
1.026
1.759/–2.113
1.012
1.131/–0.661
max/ρmin/e Å–3

Mixedꢀmetal cyclobutadienecobalt complexes
Russ.Chem.Bull., Int.Ed., Vol. 56, No. 9, September, 2007 1735
The measurements were performed in dichloromethane using
0.2 M Bu4NPF6 as the supporting electrolyte.
[Cr—Cr][Cr—Co],(Cp2Cr2(µꢀSC4H9)(µ3ꢀS)2CoCb* (5). A darkꢀ
violet solution of Cp2Cr2(µꢀSC4H9)2(µꢀS) (0.38 g, 0.85 mmol)
and 1 (0.3 g, 0.85 mmol) in benzene (35 mL) was refluxed for
2.5 h. The resulting darkꢀbrown solution was concentrated
in vacuo to 10 mL. Small needleꢀlike crystals that precipitated
after storage of the solution at 5 °C for 2 days were separated by
decantation, washed with petroleum ether (10 mL), and dried
Differential scanning calorimetry (DSC) and thermograviꢀ
metry (TG) were carried out on DSCꢀ20 and TGꢀ50 units of a
Mettler TAꢀ3000 thermoanalyzer. The experiments were perꢀ
formed under an inert atmosphere (dry argon) at a constant
heating rate of 5 deg min–1. The weight loss during heating was
monitored directly on the TGꢀ50 unit; the accuracy of the weighꢀ
ing was 2•10–3 mg. The temperatures of anomalous points in
the thermograms were determined with an accuracy of 0.5°.
Synthesis of cobalt πꢀtetramethylcyclobutadienedicarbonylꢀ
phenyltelluride, Cb*Co(CO)2TePh (2), and the dimer of cobalt
πꢀtetramethylcyclobutadienecarbonylꢀµꢀphenyltelluride,
[Cb*Co(CO)TePh]2 (3). A colorless PhTeNa solution, which
was prepared by the reaction of Na (0.33 g, 14.28 mmol) with
Ph2Te2 (0.29 g, 0.71 mmol) in THF (20 mL) at room temperaꢀ
ture for 2 h, was filtered and added to a red solution of comꢀ
pound 1 (0.50 g, 1.43 mmol) in THF (20 mL). The solution
in vacuo. The yield was 0.23 g (49%). IR (KBr), ν/cm–1
:
2920 m br, 2870 m br, 1430 m br, 1355 m, 1225 w, 1150 m,
1100 w, 1005 s, 780 v.s. Found (wt.%): C, 47.6; H, 5.6; S, 16.5.
C22H31S3Cr2Co. Calculated (wt.%): C, 47.65; H, 5.63; S, 17.34.
Crystals suitable for Xꢀray diffraction were grown by crystalꢀ
lization at the CH2Cl2—hexane interface.
This study was financially supported by the Russian
Foundation for Basic Research (Project No. 06ꢀ03ꢀ
32391), the Russian Academy of Sciences (Program
OKh 1.5), and the Council on Grants of the President of
the Russian Federation (Program for State Support of
Young Doctors, Grant MKꢀ8551.2006.3).
turned darkꢀbrown (ν
= 1970 and 1900 cm–1). The TLC
CO
pattern (Silufol, benzene) showed a red spot with Rf = 0.5,
which gradually turned colorless. The solvent was removed
in vacuo (20 Torr), and the residue was extracted with petroleum
ether (60 mL) at 30—70 °C. The brown solution was concenꢀ
trated in vacuo to 10 mL. After storage at –18 °C for 1 day,
a black precipitate of 3 was obtained. The precipitate was sepaꢀ
rated by filtration, washed with cold pentane, and dried in vacuo.
IR (νCO, CH2Cl2): 1960 cm–1. Found (wt.%): C, 45.14; H, 3.14.
C15H17OCo. Calculated (wt.%): C, 45.06; H, 4.29.
The mother liquor was concentrated in vacuo at room temꢀ
perature to 1/10 of the initial volume. After storage at –18 °C
for 1 day, redꢀblack crystals of 2 precipitated. The crystals were
filtered off, washed with cold petroleum ether (2 mL), and dried
in air over a short period of time. IR (νCO, CH2Cl2): 1970,
1900 cm–1. Since the storage of crystals of 2 in vacuo and grindꢀ
ing of the crystals with KBr led to their rapid transformation into
black product 3, the elemental composition of 2 was not deterꢀ
mined. The total yield of 2 and 3 was 0.12 g (20%). Single
crystals of 2 were studied by Xꢀray diffraction.
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(0.25 g, 0.7 mmol) and 0.7 mM sodium phenyltelluride (the
latter was prepared by the reduction of Ph2Te2 (0.7 mmol) with
a tenfold excess of sodium in THF (20 mL)). The reaction
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or dichloromethane. After removal of the solvent, the same subꢀ
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0.11 g (0.15 mmol, 22%). IR (ν/cm–1): 2060 s, 2030 s, 2000 s,
1930 s, 1430 s, 1020 s, 740 s, 690 m, 600 s, 590 s, 520 s.
Found (wt.%): C, 33.2; CO, 26.6;*; Ph, 9.1;* Me4C4, 14.2.*
C21H17O7TeCoW. Calculated (wt.%): C, 33.5; CO, 26.0;
Ph, 10.2; Me4C4, 14.3.
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13. SHELXTLꢀ97 V5.10, Bruker AXS Inc., Madison, USA, 1997.
Synthesis of dichromium πꢀtetramethylcyclobutadienecobaltꢀ
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Received June 29, 2007;
* Determined by the DSC method.
in revised form August 29, 2007