Synthesis of tellurido-bridged IrPt2, IrPd2, and IrPtPd clusters by inserting zero-valent Pt and Pd centers into Te-C bonds

Article abstract of DOI:10.1002/anie.200602203

Te for two: A convenient method to prepare a series of tellurido-bridged mixed-metal clusters is demonstrated by the reactions of [Cp*Ir(CO)(TeTol) ₂] (Tol = p-CH₃C₆H₄, Cp* = η⁵-C₅Me₅) with [Pt(PPh₃) ₃] and [Pd(PPh₃)₄]. The Group 10 metal center inserts itself into the Te-C bond (see scheme). This method may be applied to the synthesis of a wide range of mixed-metal telluride cluster compounds. (Chemical Equation Presented).

Full text of DOI:10.1002/anie.200602203

Communications
Cluster Compounds
DOI: 10.1002/anie.200602203
Synthesis of Tellurido-Bridged IrPt2, IrPd2, and
IrPtPd Clusters by Inserting Zero-Valent Pt and
À
Pd Centers into Te C Bonds**
Takafumi Nakagawa, Hidetake Seino, Shoken Nagao,
and Yasushi Mizobe*
Soluble transition-metal sulfido clusters have been investi-
gated extensively because of their relevance to biological and
industrial catalysts. In contrast, the chemistry of the analogues
of tellurium, the heavier congener of sulfur, has been less-well
developed.[1] This difference is presumably because, at least in
[*] T. Nakagawa, Dr. H. Seino, Dr. S. Nagao, Prof. Dr. Y. Mizobe
Institute of Industrial Science
The University of Tokyo
Komaba, Meguro-ku, Tokyo, 153-8505 (Japan)
Fax: (+81)3-5452-6361
E-mail: ymizobe@iis.u-tokyo.ac.jp
[**] This work was supported by Grant-in-Aid for Scientific Research on
Priority Areas (No. 14078206, “Reaction Control of Dynamic Com-
plexes”) from the Ministry of Education, Culture, Sports, Science
and Technology, Japan, and by CREST of JST.
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Chemie
part, good tellurido sources that can be used in organic media
are scarce.[2]
PhEEPh in THF by photo-irradiation. However, X-ray
structures were not determined.[14]
In the last decade, studies in our group have focused on
the pursuit of rational methods to construct metal sulfido and
selenido cluster cores with desired structures and atom
compositions.[3] In the course of these studies, we have
demonstrated that newly prepared dinuclear m-hydrosulfido
and m-hydroselenido complexes of the type [Cp*MCl(m-
EH)2MCp*Cl] (M = Ru, Ir, Rh; E = S, Se; Cp* = h5-C5Me5)
can serve as versatile building blocks to synthesize a variety of
homo- and heterometallic sulfido, selenido, and sulfido–
selenido clusters.[3,4] However, preparation of the correspond-
ing tellurido clusters is not yet feasible, as the hydrotellurido
analogues of these m-EH complexes are not accessible.
Formations of tellurido ligands from coordinated tellur-
olates have been observed for isolated or in situ-generated
complexes of Cr,[5] Mo,[6] Re,[7] Pd,[8] Ag,[9] and Cu.[10]
When 1 was treated with two equivalents of [Pt(PPh3)3] in
THF at room temperature, the mixed-metal tellurido cluster
[{Cp*Ir(CO)}(m3-Te)2{PtTol(PPh3)}2] (2) was obtained. The
NMR spectra of the residue obtained from the reaction
mixture after removal of solvent by evaporation showed the
presence of the two isomers, 2a and 2b (Scheme 1). After
À
Furthermore, cleavage of the E C bonds of organochalcogen
compounds has also been demonstrated in a well-defined
manner for the reactions with low-valent late transition
metals,[11] which include the oxidative addition reactions of
Ph2Te with zero-valent Group 10 metal complexes.[12] On the
basis of these findings, we have attempted the synthesis of
mixed-metal tellurido clusters by a new route, which involves
the initial preparation of an Ir tellurolato complex by using
readily available RTeTeR compounds (in which R = aryl) as
the Te source and subsequent transformation of this complex
À
into the tellurido clusters through Te C bond cleavage of the
tellurolato ligands by using Group 10 noble metals.
Treatment of [Cp*Ir(CO)2] with one equivalent of TolTe-
TeTol (Tol = p-CH3C6H4) in benzene at room temperature
afforded a bis(tellurolato) complex [Cp*Ir(CO)(TeTol)2] (1)
in high yield [Eq. (1)], which has been characterized by
Scheme 1. Synthetic routes for mixed-metal tellurido clusters.
crystallization of the residue from a mixture of benzene and
hexane, only the major isomer, 2a, was isolated as single
crystals and fully characterized by X-ray diffraction.[13] As
shown in Figure 2, 2a has a triangular IrPt2 core with two
capped tellurido ligands, for which, separations of Ir(1) from
Pt(1) and Pt(2) by 3.8049(5)–3.8588(6) Š as well as Pt···Pt
interatomic distances of 3.1539(6) and 3.2523(7) Š indicate
the absence of any metal–metal bonding interactions. The Ir
center has a three-legged geometry, while the geometry
around two Pt atoms is square-planar. Two phosphine ligands
are mutually trans with respect to the Pt–Pt vector, as are the
two Tol ligands. The X-ray structure was not available for 2b,
but its NMR data are analogous to those of 2a and suggest a
structure with two mutually cis-phosphine ligands (shown in
Scheme 1 for 2b). Because of steric repulsion between the
two phosphine ligands, 2b is the less-favored isomer. Note
that 2a redissolved in C6D6 and converted readily into an
equilibrium mixture of 2a and 2b at room temperature, the
ratio of which was 4:1, thus indicating that the isomerization
of 2a into 2b is fast for this IrPt2 cluster.
single-crystal X-ray analysis (Figure 1).[13] Complex 1 has an
expected three-legged structure, for which the interatomic
distances and angles are not unusual. Related thiolato and
selenolato complexes [Cp*Ir(CO)(EPh)2] (E = S, Se) are
known, which were prepared from [Cp*Ir(CO)2] and
Figure 1. An ORTEP drawing of 1. Hydrogen atoms are omitted for
clarity (thermal ellipsoids shown at 30% probability). Selected bond
lengths [Š] and angles [8]: Ir–Te(1) 2.6654(6), Ir–Te(2) 2.6579(8); Te(1)-
Ir-Te(2) 79.46(2).
Treatment of 1 with two equivalents of [Pd(PPh3)4] gave
the Pd analogue of 2, [{Cp*Ir(CO)}(m3-Te)2{PdTol(PPh3)}2]
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Figure 3. An ORTEP drawing of 4a. Hydrogen atoms are omitted for
clarity (thermal ellipsoids shown at 30% probability). Selected bond
lengths [Š] and angles [8]: Ir···Pt 3.9198(5); Ir-Te(1)-Pt 95.98(2), Ir-
Te(2)-Pt 95.50(2), Te-Ir-Te 76.38(2), Te-Pt-Te 77.42(2).
Figure 2. An ORTEP drawing of 2a. Only one of the two independent
molecules is shown (thermal ellipsoids shown at 30% probability). For
clarity all the hydrogen atoms are omitted and only the carbon atom
bound to P is shown for the phenyl groups of the PPh3 units. Selected
bond lengths [Š] and angles [8]: Ir–Te 2.6769(7)–2.6985(7), Pt–Te,
2.6347(8)–2.7052(7); Ir-Te-Pt, 89.82(2)–92.69(2), Pt-Te-Pt, 72.39(2)–
75.23(2), Te-Ir-Te 75.26(2), 75.60(2), Te-Pt-Te, 75.86(2)–76.44(2). In
isostructural 3a: Ir···Pd 3.784(1)–3.837(1), Pd···Pd 3.185(2), 3.089(1),
Ir-Te, 2.666(1)–2.689(1), Pd-Te, 2.605(1)–2.702(2), Ir-Te-Pd 89.49(4)–
92.91(3), Pd-Te-Pd, 71.31(4)–74.12(4), Te-Ir-Te 75.68(3), 75.91(3), Te-
Pd-Te, 76.60(4)–76.98(4).
Figure 3). Unfortunately, an X-ray crystal structure was not
obtainable for 4b. However, spectroscopic data of 4b are
consistent with the structure shown in Scheme 1, in which
only the geometry around Pt differs from that of 4a. Complex
4a dissolved in C6D6 and converted into a 2.2:1 mixture of 4a
and 4b in equilibrium after 30 h at room temperature. A
similar isomerization was reported for the reaction of [Pt-
(PEt3)3] with iPrTePh, in which the initial product cis-[PtPh-
(TeiPr)(PEt3)2] transformed smoothly into trans-[PtPh-
(TeiPr)(PEt3)2].[11] Treatment of an equilibrium mixture of
4a and 4b with one equivalent of [Pt(PPh3)3] afforded a
mixture of 2a and 2b, which indicates that the complexes 4
are the intermediates in the reaction course of 1 to 2.
It is noteworthy that from the reaction of 1 with [Pd-
(PPh3)4], the telluride–tellurolato complex corresponding to 4
was not obtained. The reaction of equimolar 1 and [Pd-
(PPh3)4] resulted in the formation of a mixture of the
trinuclear tellurido cluster, 3, and residual 1, as indicated by
the NMR spectra of the reaction mixture recorded soon after
mixing.
(3), which is present as a mixture of 3a and 3b under the
reaction conditions (Scheme 1). Workup of the product
solution afforded only 3a as single crystals and the X-ray
analysis disclosed its structure to be analogous to that of 2a.[13]
When redissolved in C6D6, 3a slowly converted into an
equilibrium mixture of 3a and 3b to reach a molar ratio of 3:1.
This isomerization of the IrPd2 cluster is considerably slower
than that of the IrPt2 cluster, 2a. As addition of 0.1 equiv-
alents of PPh3 to the solution of 3a significantly decreases the
rate of the formation of 3b, this isomerization presumably
proceeds through dissociation of PPh3. The much-faster
isomerization of 2a than that of 3a may be ascribable to the
higher ability of PPh3 to dissociate from a Pt center than from
a Pd center.
The reaction of 1 with one equivalent of [Pt(PPh3)3] in
THF at room temperature resulted in the isolation of the
intermediate in the conversion of 1 into 2. Workup of the
reaction mixture afforded the tellurido- and tellurolato-
bridged dinuclear complex [Cp*Ir(CO)(m-Te)(m-TeTol)PtTol-
(PPh3)] (4), which was isolated as a mixture of isomers, 4a and
4b (Scheme 1). For the major isomer, 4a, the structure has
been determined unambiguously by X-ray analysis of single
crystals obtained after repeated crystallization of this mixture
(Figure 3).[13] Two metal centers are connected by one m-
telluride and one m-tellurolate, in which the tellurido and Tol
ligands around Pt are mutually cis. Oxidative addition of a Pt0
It was also found that from the reaction of the Ir–Pt
complex, 4, with [Pd(PPh3)4], another trinuclear cluster
[{Cp*Ir(CO)}(m3-Te)2{PtTol(PPh3)}{PdTol(PPh3)}] (5) was
available through the facile insertion of a Pd0 center into
À
the remaining Te Tol bond in complex 4 (Scheme 1). The
NMR spectra of the reaction mixture showed the presence of
5a. After removal of the solvent by evaporation, crystalliza-
tion of the residue from a mixture of THF and hexane
afforded 5a as single crystals. The NMR spectra of 5a in C6D6
indicated its rapid transformation into an equilibrium mixture
of 5a and 5b in a 3:1 molar ratio. The X-ray crystal structure
of 5a is depicted in Figure 4.[13] Cluster 5a has the expected
triangular core capped by two m3-tellurido ligands, in which
the Pd atom occupies the vertex close to the CO ligand,
presumably because the insertion of the Pd center into the
À
center across one Te Tol bond in 1 and coordination of a Te
atom of the other intact TeTol ligand to Pt affords 4a. There
are no bonding interactions between metal centers in 4a. The
À
Te Tol bond occurs selectively at the sterically less-crowding
À
Pt Te(1) bond at 2.6563(7) Š is considerably longer than the
side with respect to the IrPtTe2 core in 4, namely, from the
direction opposite the Cp* ligand. Two PPh3 ligands are
mutually trans as observed for 2a and 3a, and similarly the
structure of 5b may be assigned as that with two PPh3 ligands
mutually cis around the Pt···Pd vector.
À
Pt Te(2) bond at 2.6013(7) Š presumably because of the
strong trans influence exerted by the Tol ligand. Around the Ir
À
center, the Ir-m-tellurolato bond (Ir Te(1) 2.6243(6) Š) is
À
shorter than the Ir-m-tellurido bond (Ir Te(2) 2.6934(8) Š;
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presence of two products, 2a and 2b, in a molar ratio of 2:1.
Crystallization of the residue from a mixture of benzene and hexane
(1:10) afforded pure 2a·0.25C6H6 as red crystals (43 mg, 48% yield).
Complex 2a dissolved in C6D6 and converted into an equilibrium
mixture of 2a and 2b in the ratio of 4:1. 2a: IR (KBr): n˜ = 1979 cmÀ1
,
n(CO); 1H NMR (C6D6): d = 1.70 (s, 15H, Cp*), 2.15, 2.21 (s, 3H
each, Me in Tol), 6.73, 6.85, 7.53, 7.60 (d, J = 7.6 Hz, 2H each, C6H4),
7.0–7.1 (m, 18H, Ph), 7.8–8.0 ppm (m, 12H, Ph); 31P{1H} NMR
(C6D6): d = 7.1 (d with 195Pt satellites, JP–P = 5 Hz, JPt–P = 3790 Hz),
7.4 ppm (d with 195Pt satellites, JP–P = 5 Hz, JPt–P = 3700 Hz); elemental
analysis (%) calcd for C62.5H60.5OIrP2Pt2Te2: C 43.46, H 3.53; found:
1
C 43.65, H 3.52. Data assignable to 2b: H NMR (C6D6): d = 1.71 (s,
15H, Cp*), 2.14, 2.16 ppm (s, 3H each, Me in Tol); 31P{1H} NMR
(C6D6): 6.6 (d with 195Pt satellites,
JP-P = 8 Hz, JPt-P = 3770 Hz),
6.9 ppm (d with 195Pt satellites, JP–P = 8 Hz, JPt-P = 3930 Hz).
3: [Pd(PPh3)4] (116 mg, 0.100 mmol) was added to a THF solution
(5 mL) of 1 (40 mg, 0.050 mmol) and the resultant black solution was
stirred at room temperature for 23 h. The NMR spectrum of the
reaction mixture showed the presence of two isomeric products, 3a
and 3b, in a 3:1 ratio. Hexane was added to the concentrated product
solution and kept at À208C to yield black crystals of 3a·0.25C6H14
(32mg, 41% yield). When redissolved in C 6D6, 3a was converted very
slowly into an equilibrium mixture of 3a and 3b. The rate constants
for the conversion of 3a into 3b and its reverse reaction at 293 K were
calculated to be 4.5 ” 10À5 sÀ1 and 13 ” 10À5 sÀ1, respectively, based on
the 1H NMR spectral change. IR (KBr): n˜ = 1971 cmÀ1, n(CO);
elemental analysis (%) calcd for C62.5H62.5OIrP2Pd2Te2: C 48.37;
H 4.06; found: C 47.64, H 3.83. Data assignable to 3a: 1H NMR
(C6D6): d = 1.71 (s, 15H, Cp*), 2.14, 2.23 (s, 3H each, Me in Tol), 6.73,
6.78, 7.40, 7.48 (d, J = 8.0 Hz, 2H each, C6H4), 7.0–7.1 (m, 18H, Ph),
7.8–8.0 ppm (m, 12H, Ph); 31P{1H} NMR (C6D6): d = 14.7 (d, J =
7 Hz), 14.9 ppm (d, J = 7 Hz). Data assignable to 3b: 1H NMR
(C6D6): d = 1.75 (s, 15H, Cp*), 2.13, 2.16 ppm (s, 3H each, Me in Tol);
31P{1H} NMR (C6D6): d = 14.7 (d, overlapping with the signal of 3a),
15.5 ppm (d, J = 8 Hz).
Figure 4. An ORTEP drawing of 5a. Only one of the two independent
molecules is shown (thermal ellipsoids shown at 30% probability). For
clarity all the hydrogen atoms are omitted and only the carbon atom
bound to P is shown for the phenyl groups of the PPh3 units. Selected
bond lengths [Š] and angles [8]: Ir···Pt, 3.8534(6), 3.8505(6), Ir···Pd
3.7821(8), 3.7879(7), Pt···Pd 3.2002(9), 3.1053(7), Ir-Te 2.6712(8)–
2.6870(8), Pt-Te 2.6162(8)–2.6827(8), Pd-Te 2.6179(9)–2.718(1), Ir-Te-
Pt 91.72(2)–93.52(2), Ir-Te-Pd 89.22(3)–91.47(3); Pt-Te-Pd, 71.39(2)–
74.34(2), Te-Ir-Te 75.43(2), 75.85(2), Te-Pt-Te 76.44(2), 76.72(2), Te-Pd-
Te 75.88(3), 76.55(2).
In conclusion, a versatile route for synthesizing mixed-
metal tellurido clusters in solution has been developed, which
involves the use of a readily available tellurolato complex as a
4: A mixture of 1 (160 mg, 0.202 mmol) and [Pt(PPh3)3] (200 mg,
0.204 mmol) in THF (5 mL) was stirred at room temperature for one
day and the resultant dark green solution was evaporated to dryness
in vacuo. The 1H NMR spectra of the residue showed the presence of
the products 4a and 4b in a molar ratio of 3:1. The residue was
extracted with benzene and the addition of hexane to the concen-
trated extract afforded a 3:1 mixture of 4a and 4b as dark green
crystals (177 mg, 70% combined yield). Single crystals of pure 4a
were obtained by repeated fractional crystallization from a mixture of
benzene and hexane. 4a was dissolved in C6D6 and allowed to stand
for 30 h at room temperature; the resulting solution contained a
mixture of 4a and 4b in equilibrium in a ratio of 2.2:1 as confirmed by
1H NMR spectroscopy. IR (KBr): n˜ = 1991 cmÀ1, n(CO); elemental
analysis (%) calcd for C43H44OIrPPtTe2: C 41.31, H 3.55; found:
À
metal–tellurido building block through Te C bond scission
with M0 centers (M = Pt, Pd). Note that the reactions of 1 with
PtII and PdII complexes [MCl2(cod)] (cod = cyclooctadiene)
result in the formation of only the tellurolato-bridged
dinuclear and trinuclear complexes [Cp*Ir(CO)(m-
TeTol)2MCl2] (M = Pt, Pd) and [{Cp*Ir(CO)(m-TeTol)2}2Pt],
which will be described elsewhere. Application of the method
reported herein to the synthesis of a wide range of mixed-
metal tellurido clusters is now in progress.
1
C 41.06, H 3.69. Data assignable to 4a: H NMR (C6D6): d = 1.63 (s,
Experimental Section
15H, Cp*), 1.97, 2.10 (s, 3H each, Me in Tol), 6.59, 7.19, 7.39,
7.71 ppm (d, J = 8.0 Hz, 2H each, C6H4); 31P{1H} NMR (C6D6): d =
9.5 ppm (s with 195Pt satellites, JPt-P = 3910 Hz). Data assignable to 4b:
1H NMR (C6D6): d = 1.68 (s, 15H, Cp*), 1.97, 2.12 ppm (s, 3H each,
Me in Tol); 31P{1H} NMR (C6D6): d = 20.4 ppm (s with 195Pt satellites,
All manipulations were carried out under an atmosphere of N2 by
using Schlenk techniques. Complexes [Cp*Ir(CO)2],[15] [Pt(PPh3)3],[16]
[Pd(PPh3)4],[17] and TolTeTeTol[18] were prepared by reported meth-
ods.
1: TolTeTeTol (230 mg, 0.526 mmol) was added to a solution of
[Cp*Ir(CO)2] (191 mg, 0.498 mmol) in benzene (10 mL) at room
temperature. The reaction mixture was stirred for 3 h at room
temperature and the resultant deep red solution was concentrated
in vacuo. Addition of hexane afforded 1 as deep red crystals (315 mg,
JPt-P = 3900 Hz).
5: [Pd(PPh3)4] (58 mg, 0.050 mmol) was added to a THF solution
(5 mL) of 4a and 4b (65 mg, 0.052mmol) and this mixture was stirred
for 5 h at room temperature. The NMR spectra of the reaction
mixture showed the presence of 5a. Addition of hexane to the
concentrated product solution afforded 5a·0.25C6H14 as red crystals
(40 mg, 46% yield). When dissolved in C6D6, 5a converted into an
equilibrium mixture of 5a and 5b at room temperature, the ratio of
which was 3:1. IR (KBr): n˜ = 1968 cmÀ1, n(CO); elemental analysis
(%) calcd for C62.5H62.5OIrP2PdPtTe2: C 45.76, H 3.84; found: C 45.55,
H 3.76. Data assignable to 5a: 1H NMR (C6D6): d = 1.72(s, 15H,
Cp*), 2.13, 2.21 (s, 3H each, Me in Tol), 6.72, 6.86, 7.38, 7.65 (d, J =
1
79% yield). IR (KBr): n˜ = 1982cm À1, n(CO); H NMR (C6D6): d =
1.55 (s, 15H, Cp*), 2.06 (s, 6H, Me in Tol), 6.75, 7.96 ppm (d, J =
7.9 Hz, 4H each, C6H4); elemental analysis (%) calcd for
C25H29OIrTe2: C 37.87, H 3.69; found: C 37.51, H 3.53.
2: [Pt(PPh3)3] (101 mg, 0.103 mmol) was added to a THF solution
(5 mL) of 1 (41 mg, 0.051 mmol) and the mixture was stirred for 26 h
at room temperature. The resultant red solution was evaporated to
dryness in vacuo. The 1H NMR spectrum of this residue indicated the
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7.6 Hz, 2H each, C6H4), 7.0–7.1 (m, 18H, Ph), 7.8–8.0 ppm (m, 12H,
Ph); 31P{1H} NMR (C6D6): d = 11.0 (d with 195Pt satellites, JP-P = 6 Hz,
2.048 gcmÀ3, R1 = 0.0360 (3428 data with I > 2s(I)) and wR2 =
0.0970 (all 5887 unique data) for 291 variables, GOF = 1.031.
2a·0.25C6H6: Mr = 1727.21, 0.40 ” 0.20 ” 0.10 mm3, triclinic,
JPt-P = 3650 Hz), 11.9 ppm (d, JP-P = 6 Hz). Data assignable to 5b:
1H NMR (C6D6): d = 1.69 (s, 15H, Cp*), 2.15, 2.23 ppm (s, 3H each,
Me in Tol); 31P{1H} NMR (C6D6): d = 10.8 (d, JP-P = 6 Hz; 195Pt
satellites could not be resolved), 11.4 ppm (d, JP-P = 6 Hz).
space group P1, a = 14.987(3), b = 18.459(4), c = 22.293(5) Š,
¯
a = 97.113(3), b = 102.993(3), g = 96.124(3)8, V= 5905(2) Š3,
Z = 4, room temperature, 1calcd = 1.943 gcmÀ3
, R1 = 0.0380
X-ray crystallography: Single crystals of 1, 2a·0.25C6H6,
3a·0.25C6H14, 4a, and 5a·0.25C6H14 were sealed in glass capillaries
under argon and mounted on a Rigaku Mercury-CCD diffractometer
equipped with a graphite-monochromatized MoKa source. All dif-
fraction studies were carried out at room temperature.
Structure solution and refinements were carried out by using the
CrystalStructure program.[19] The positions of the non-hydrogen
atoms were determined by Patterson methods (PATTY[20]) and
subsequent Fourier synthesis (DIRDIF 99[21]). Non-hydrogen atoms
were refined anisotropically by minimizing wR2based on all data, for
which full-matrix least-squares techniques are employed. All hydro-
gen atoms were placed at the calculated positions and included at the
final stages of the refinements with fixed parameters.
(17619 data with I > 2s(I)) and wR2 = 0.1290 (all 26675
unique data) for 1351 variables, GOF = 1.019. 3a·0.25C6H14:
3
¯
Mr = 1551.85, 0.20 ” 0.10 ” 0.05 mm , triclinic, space group P1,
a = 14.966(6), b = 18.422(6), c = 22.259(9) Š, a = 97.023(5), b =
103.306(6), g = 95.816(5)8, V= 5874(4) Š3, Z = 4, room temper-
ature, 1calcd = 1.755 gcmÀ3, R1 = 0.0660 (10818 data with I >
2s(I)) and wR2 = 0.1930 (all 25822 unique data) for 1395
variables, GOF = 1.008. 4a: Mr = 1250.30, 0.50 ” 0.15 ”
0.02mm 3, monoclinic, space group P21/a, a = 17.857(3), b =
10.702(2), c = 22.276(4) Š, b = 104.8625(7)8, V= 4115(1) Š3,
Z = 4, room temperature, 1calcd = 2.018 gcmÀ3
(6319 data with I > 2s(I)) and wR2 = 0.1300 (all 9381 unique
data) for 486 variables, GOF = 1.004. 5a·0.25C6H14 Mr =
, R1 = 0.0410
:
3
¯
1640.54, 0.30 ” 0.25 ” 0.15 mm , triclinic, space group P1, a =
14.939(2), b = 18.439(3), c = 22.229(3) Š, a = 96.981(2), b =
103.311(2), g = 95.562(2)8, V= 5865(2) Š3, Z = 4, room temper-
ature, 1calcd = 1.858 gcmÀ3, R1 = 0.0560 (16567 data with I >
2s(I)) and wR2 = 0.1650 (all 25735 unique data) for 1355
variables, GOF = 1.027. CCDC-616845–616849 (1, 2a, 3a, 4a,
and 5a, respectively) contain the supplementary crystallographic
data for this paper. These data can be obtained free of charge
from The Cambridge Crystallographic Data Centre via
www.ccdc.cam.ac.uk/data_request/cif.
Received: June 2, 2006
Revised: August 9, 2006
Published online: October 19, 2006
Keywords: cluster compounds · iridium · palladium · platinum ·
.
tellurium
[1] a) J. Wachter, Eur.J.Inorg.Chem. 2004, 1367; b) D. Fenske, J. F.
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[13] X-ray data for 1: Mr = 792.92, 0.20 ” 0.10 ” 0.10 mm3, monoclinic,
space group P21/n, a = 7.815(2), b = 12.696(3), c = 26.055(6) Š,
b = 95.889(1)8, V= 2571(1) Š3, Z = 4, room temperature, 1calcd
=
7762
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