Phosphorus-centered and phosphinidene-capped tungsten chloride clusters

Article abstract of DOI:10.1002/ejic.201100122

Black crystalline powders of W₆PCl₁₇ and W ₄(PCl)Cl₁₀ were obtained after reducing WCl₆ with red phosphorus at 370 and 500 °C. The crystal structures were determined by single-crystal and powder X-ray

Full text of DOI:10.1002/ejic.201100122

FULL PAPER
DOI: 10.1002/ejic.201100122
Phosphorus-Centered and Phosphinidene-Capped Tungsten Chloride Clusters
[a]
[b]
[a]
Markus Ströbele, Klaus Eichele, and H.-Jürgen Meyer*
Dedicated to Professor John D. Corbett on the occasion of his 85th birthday
Keywords: Tungsten / Cluster compounds / Solid-state structures / X-ray diffraction
Black crystalline powders of W
obtained after reducing WCl
and 500 °C. The crystal structures were determined by sin-
gle-crystal and powder X-ray diffraction analyses. The struc-
6
PCl17 and W
with red phosphorus at 370
4
(PCl)Cl10 were
ture of W
4
(PCl)Cl10 is represented by a Jahn–Teller distorted
6
tetranuclear tungsten cluster that is interconnected into a
layered [W
chloro-phosphinidene ligand. Solid-state P magic-angle
spinning (MAS) NMR spectra, electronic structures, and
magnetic properties are reported.
i
a–a
4
(μ
4
-PCl)Cl
6
]Cl8/2
structure containing
a
3
1
ture of W
6
PCl17 is represented by a phosphorus-centered
a
a–a
hexanuclear tungsten cluster, whose (W
6
PCl11)Cl Cl4/2
4
chains form a hexagonal stick packing structure. The struc-
Introduction
muth has opened up an alternative route for the synthesis
[
10]
of W Cl .
6
12
The chemistry of transition-metal clusters is a unique
field of chemistry with inherently beautiful cluster motifs, a
surprising chemistry in solid state and in solution, and with
developing applications. One of the most simple tungsten
W Cl itself is an attractive starting material for the
6
12
preparation of other cluster compounds, as shown by
oxidation and reduction reactions with carbon halide
sources. Various tungsten halide clusters can be obtained,
among them the novel compounds W C (Cl,Br) and
chloride cluster compounds is W Cl with an octahedral
6
12
30
2
68
cluster core, which represents the functional block for its
[11]
W CCl .
6
15
[
1]
remarkable properties with regard to photoluminescence,
At present, we are exploring the reduction of WCl by
6
[
2]
[3]
catalysis, and chemical sensing.
Besides the polymeric structure of W Cl {or (W Cl )-
using soft reducing agents and moderate heating tempera-
tures (this temperature region is not often used) in order to
explore the potentially largest field of missing compounds –
i
6
12
6
8
a
a–a
Cl Cl
}, there are two molecular-based structures of
2
4/2
tungsten chloride clusters, namely octahedro-W Cl
[12]
6
18
the thermally labile cluster compounds.
i
a [4]
{(W CCl i)-
{
(W Cl )Cl }
and triprismo-W CCl
6
12
[5]
6
6 18
6
12
Over the course of systematic investigations with the em-
ployment of phosphorus as a reducing agent, we here pres-
ent the novel cluster compounds W PCl and W (PCl)Cl ,
a
Cl }. The structure of W CCl contains a carbon-cen-
6
6
18
tered trigonal-prismatic cluster and follows the prototype
6
17
4
10
[6]
structure of A [Nb SBr ] (A = K, Rb, Cs, Tl) with a
3
6
17
which represent the first examples of phosphorus-contain-
sulfur-centered trigonal-prismatic cluster core.
Most tungsten halide clusters like octahedro-[W Cl ]
ing tungsten halide clusters. The WCl reduction with ele-
6
n–
6
18
mental red phosphorus has been described before, but obvi-
m–
and triprismo-[W ZCl ] with Z = C or N can be em-
[13,14]
6
18
ously under different conditions.
[
7]
ployed in solution chemistry with variable oxidation states
and diverse ligands.[
8]
Results and Discussion
The synthesis of metal-rich tungsten chlorides is usually
performed following the reduction of WCl with electropos- Synthesis and Characterization
6
itive metals; the reduction with aluminium is well-estab-
The phosphorus-centered cluster compound W PCl is
formed as a black microcrystalline powder by reduction of
6
17
[
9]
lished. Recently, the reduction of WCl with the metal bis-
6
WCl with elemental red phosphorus at around 360–380 °C.
6
[
[
a] Institut für Anorganische Chemie, Abteilung für
Festkörperchemie und Theoretische Anorganische Chemie,
Universität Tübingen,
The slightly more reduced phosphinidene-capped tetranu-
clear cluster compound W (PCl)Cl was obtained at
4
10
Ob dem Himmelreich 7, 72074 Tübingen, Germany
E-mail: juergen.meyer@uni-tuebingen.de
500 °C and forms black plate-like crystals. The structures
of these compounds contain an interstitial phosphido and
a capping phosphinidene ligand, which are both known as
important and versatile ligands in organic chemistry and as
b] Institut für Anorganische Chemie, Universität Tübingen,
Auf der Morgenstelle 18, 72076 Tübingen, Germany
E-mail: klaus.eichele@uni-tuebingen.de
Eur. J. Inorg. Chem. 2011, 4063–4068
© 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
4063

M. Ströbele, K. Eichele, H.-J. Meyer
FULL PAPER
nucleating ligands in metal cluster chemistry. These ligands dination mode of the phosphorus atom in these compounds
enhance the structural integrity and stability through their is μ -capping and the P atom is treated as a phosphido li-
3
3
–
characteristic face-capping coordination capabilities.
The presence of an interstitial phosphorus atom appears
gand (P ).
When the phosphorus atom in W PCl is treated in the
6
17
to be rare in the chemistry of metal halide clusters, in con- same way, an electron count of 16 electrons per W core can
6
trast to the well-known presence of interstitial carbon or be assigned. This electron count is consistent with results
nitrogen atoms. The only example known to us is the series of an extended Hückel molecular orbital calculation of an
2–
of (M )Zr I P (M = Rb, Cs) compounds developed by isolated [W PCl ] cluster. EHMO calculations are known
z
6 14
6
19
Corbett and co-workers, where the phosphorus atom re- to be inherently semiempirical and qualitative, but show
[
18]
sides in the center of an octahedral zirconium cluster good results in cluster chemistry.
[
The total electron
dZr–P = 2.432(2) and 2.494(1) Å].[
15]
2–
count of 176 valence electrons of an isolated [W PCl ]
6 19
From a structural point of view, a phosphorus-centered cluster is confined in 80 energetically low-lying anionic en-
tungsten cluster may be expected to be related to the known ergy levels (3s and 3p levels of Cl and P) and eight metal-
carbon-centered triprismo-W CCl18 cluster or to the motive centered energy levels, with a nearly nonbonding HOMO.
6
of a centered octahedro cluster, known as an empty cluster
in W Cl . Actually, the refined crystal structure of distinction to carbon-centered octahedral metal clusters of
Following this assignment of electrons, we note a clear
6
18
n–
W PCl can be considered to represent an intermediate the [Zr CCl ] -type, where strong interactions between
6
17
6
18
cluster species in-between an octahedral and a trigonal-pris- carbon 2s, 2p orbitals and cluster d orbitals yield four
b
b
matic cluster, having eight short W–W contacts. A compari- bonding energy levels [(a –a ) , (t –t ) ] below and four
1g
1g
1u 1u
son of the structures of W CCl , W PCl , and W Cl is antibonding energy levels [(a –a )*, (t –t )*] above the
6
18
6
17
6
18
1g 1g
1u 1u
displayed in Figure 1.
fermi energy. The total number of bonding cluster states
therefore remains the same, whereas the number of valence
electrons increases by four electrons by the interstitial car-
bon atom.
The weakly paramagnetic behavior obtained for W PCl
6
17
may be attributed to a very small band gap and the black
body color (metallic lustre) of the crystal powder, but an
influence of a paramagnetic impurity beyond the detection
level of X-ray powder diffraction cannot be ruled out. Phos-
phorus-31 solid-state magic angle spinning (MAS) NMR
spectra of W PCl reveal a very broad (4700 Hz fwhh)
Figure 1. Comparison of structures containing hexanuclear tung-
6
17
2
–
sten chloride clusters: W
6 6 6
CCl18, W PCl17 {shown as (W PCl19) },
asymmetric isotropic signal at δ = 41 ppm.
and W Cl18 (from left to right).
6
Tungsten atoms in the structure of W PCl have essen-
6
17
Phosphorus-containing clusters are also known in homo- tially two types of coordination environments, which can be
leptic alkoxide cluster compounds, such as the trigonal related to the coordination environments of tungsten atoms
[
16]
n–
[19]
tungsten cluster compound W (P)(OR)9
2
[dW–P
=
in the [W Cl ] (n = 2, 3) anion and in the WCl struc-
3
2
9
4
[
20]
.365(4) Å] and the rhomboidal tungsten cluster compound ture.
Nearest W–W distances in W PCl rank between
6 17
W (P) (OR) [dW–P = 2.292(4) to 2.692(1) Å].[ The coor- 2.584(3) and 3.019(4) Å (Table 1) and are very similar to
17]
4
2
10
6 4
Table 1. Interatomic distances within the crystal cores of W PCl17 and W (PCl)Cl10 in comparison with some other systems.
Compound
M–M distances / Å
2.757(3) [W(1)–W(1)]
W–P distances / Å
P–Cl distances / Å
W
6
PCl17
2.52(2) [W(1)–P(1) 2ϫ]
2.386(7) [W(2)–P(1) 2ϫ]
2.33(2) [W(3)–P(1) 2ϫ]
3.019(4) [W(1)–W(2) 4ϫ]
2.816(8) [W(2)–W(3) 2ϫ]
2.584(3) [W(3)–W(3)]
W
4
(PCl)Cl10
2.615(1) [W(1)–W(1)]
2.366(4) [W(1)–P(1) 2ϫ]
2.413(4) [W(2)–P(1) 2ϫ]
2.033(8)
2
2
.809(1) [W(1)–W(2) 2ϫ]
.623(1) [W(2)–W(2)]
PCl
PCl
3
5
2.018(3)–2.034(2)
1.903(5)–2.16(1)
[
16]
W
3
4
(P)(OR)
(P)
(OR)10[17]
9
2.757(1)
2.365(4)
W
2
2.6938(8)
2.292(4)
2.484(4)
2.7981(8)
2
2
.377(4)
.692(1)
[
22]
Mo
4
Cl
4
(OPr)
8
2.378(2) [Mo(1)–Mo(2)]
.407(3) [Mo(2)–Mo(2)Ј]
2
4064
www.eurjic.org
© 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
Eur. J. Inorg. Chem. 2011, 4063–4068

Phosphorus-Centered and Phosphinidene-Capped Tungsten Chloride Clusters
4
corresponding distances in triprismo-[W ZCl ] cluster atoms to form a (4 ) layer structure, displayed in Figure 3.
6
18
compounds [2.6518(6)–3.0705(7) Å].[ Likewise, the range Alternating layers are linked by van der Waals attractions,
of W–P distances between 2.33(2) and 2.52(2) Å is in line whereupon empty rectangular spaces within one layer are
with corresponding distances in W (P)(OR) [2.365(4) Å], filled by chloro-phosphinidene ligands of adjacent layers,
21]
3
9
W (P) (OR)
[2.292(4)–2.692(1) Å], and with PCl3 following a key–lock system.
Table 1). However, these W–P distances are expectedly
longer than the W–Z distances in triprismo-[W ZCl ] clus-
4
2
10
(
6
18
ter compounds, which typically range between 2.15 and
2.18 Å for Z = C and N.
The complete crystal structure of W PCl features a
6
17
hexagonal stick packing of halide bridged (W PCl )-
6
11
a
a–a
Cl Cl
cluster chains running parallel to the a axis (see
4
4/2
Figure 2).
4 4
Figure 3. Projection of one layer of the crystal structure of {W (μ -
i
a–a
PCl)Cl
6
}Cl8/2
.
The most remarkable feature of W (PCl)Cl is the pres-
4
10
ence of the μ -capping chloro-phosphinidene ligand, having
4
W–P distances of 2.366(4) and 2.413(4) Å, and a P–Cl dis-
tance of 2.033(8) Å, which corresponds well with the dis-
tances reported for PCl3.
Distances within the tungsten cluster cores are listed in
Table 1 and can be assigned with the labeling scheme of the
cluster cores given in Figure 4.
Figure 2. Crystal structure of (W
of a cluster chain (top) and a hexagonal stick packing of chains
PCl11)Cl aCl4/2a–a with a section
6 4
(bottom) running parallel to the a axis.
Transition of W PCl into W (PCl)Cl occurs at T Ն
6
17
4
10
380 °C and can be considered as a reduction because of
the presence of excess elemental phosphorus. The crystal
structure of W (PCl)Cl features a Jahn–Teller distorted
4
10
rectangular W -cluster core following the motif of the buta-
4
diene structure. Similar clusters were obtained for Mo X -
4
4
(
OPr) with X = Cl and Br having planar and butterfly-
8
type Mo -cluster cores, whose individual cluster arrange-
4
ments were explained simply on the grounds of crystal
[
22]
packing.
nearly) rectangular cluster core of W (PCl)Cl
Distances between tungsten atoms within the
(
are
4
10
2
.615(1), 2.623(1), and 2.809(1) Å; intercluster contact dis-
i
a–a
tances within the layers of {W (μ -PCl)Cl }Cl
are
4
4
6
8/2
3.7648(9) and 3.7756(9) Å. Following these contacts, the
Figure 4. Building blocks from structures of W
6
PCl17 (top) and
rectangular clusters are interconnected by bridging chloride
W
4
(PCl)Cl10 (bottom) with atom labels.
Eur. J. Inorg. Chem. 2011, 4063–4068
© 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.eurjic.org 4065

M. Ströbele, K. Eichele, H.-J. Meyer
FULL PAPER
[
27]
In this context, it is interesting to note that a compound bond. With these parameters fixed, the simulation
(Fig-
containing chlorocarbyne-bridged W units has been re- ure 6a) of the 31P MAS spectra yields an indirect spin–spin
2
[23]
1
35
31
35
ported as W (μ -CCl)Cl .
The chlorocarbyne ligand in coupling constant J ( Cl, P) of –155 Hz and a Cl nu-
2
2
7
iso
3
–
this compound is considered as a (CCl) anion, and tung- clear quadrupole coupling constant of –50 MHz. The mag-
5
+
sten atoms are represented as W . The chloro-phosphinid- nitude of the nuclear quadrupole coupling constant is in
ene ligand of W (PCl)Cl can be treated in an analogous line with the proposed correlation between 35Cl nuclear
4
10
manner and can be considered as a (PCl)2 anion. This view quadrupole resonance (NQR) frequencies and the P–Cl
–
[
28]
is consistent with the calculated MO scheme of an isolated bond length in chlorocyclotriphosphazatrienes.
Param-
4
–
31
37
[
W (PCl)Cl ] cluster, which reveals 63 anionic energy eters for the P, Cl spin pair have been calculated from
4
14
levels and 6 metal-based W–W bonding energy levels occu- those of the 31P, 35Cl spin pair by using the ratios of the
pied by 12 electrons (Figure 5). The (PCl) ligand is repre- magnetogyric ratios, 0.8475, or the nuclear quadrupole mo-
sented by eight orbitals (2ϫ3s + 6ϫ3p). The covalent P– ments, 0.7874. The 31P MAS spectrum at 11.75 T also exhi-
Cl interaction results in one bonding σ combination below bits several spinning sidebands (Figure 6b) caused mainly
and one antibonding σ combination above the HOMO by chemical shift anisotropy, with principal components of
level. Therefore, the total number of occupied anionic en- δ11 = 406, δ22 = 340, and δ33 = 302 ppm. In this analysis,
–
ergy levels is 14ϫ4 (Cl ) + 7 (PCl) = 63. The total electron
4
–
count of 138 valence electrons per [W (PCl)Cl ] results
4
14
in 69 occupied energy levels and 6 occupied metal-centered
states.
Figure 5. MO scheme of metal-centered states (all a levels) of an
4–
isolated [W
4
(PCl)Cl14
]
s
anion having C symmetry (ideal sym-
metry: C2v) including the bonding (+) and antibonding (–) nature
of W–W states.
This cluster electron count and the Jahn–Teller distorted
rectangular tungsten cluster core can be related to the elec-
tronic situation found in a butadiene molecule or in the
cluster core in Mo Cl (OPr) , and other tetranuclear
4
4
8
1
2+
[24]
(M4)
clusters.
Magnetic measurements on W (PCl)-
4
Cl10 reveal diamagnetic properties.
The presence of a P–Cl bond in W (PCl)Cl10 results in
4
characteristic magnetic-field-dependent splittings as de-
3
1
tected in the P MAS NMR spectra (Figure 6a). Analo-
3
1
gous splittings have been observed in the P MAS NMR
spectra of chloro derivatives of phosphazenes[ and have
been analyzed in detail to reveal underlying information on
25]
Figure 6. (a) Dependence of the isotropic peak in 31P MAS spectra
of W (PCl)Cl10 on external magnetic field strength. For both mag-
netic field strengths, experimental spectra are shown on top over
Cl nuclear quadrupole interactions. In the convoluted and unconvoluted (bottom) simulated spectra. Fre-
3
1
35/37
4
P to
well as on the
the present case, the P to Cl direct dipole–dipole cou- quencies are given relative to the isotropic chemical shift of
Cl direct and indirect spin–spin interactions as
3
5/37
[26]
3
1
35
3
1
3
4
49.5 ppm. (b) P MAS NMR spectrum of W (PCl)Cl10 at 11.75 T
pling constant has been fixed at 570 Hz and the value calcu-
lated from the P–Cl distance and the asymmetry parameter
of the electric field gradient tensor about chlorine is as-
and a spinning rate of 4 kHz. The experimental spectrum (top) was
convoluted by a Lorentzian of 500 Hz width to “hide” the fine
structure shown in (a). The bottom spectrum was calculated using
3
1
sumed to be close to zero and oriented parallel to the P–Cl the P chemical shift anisotropy parameters given in the text.
4
066 Eur. J. Inorg. Chem. 2011, 4063–4068
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© 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

Phosphorus-Centered and Phosphinidene-Capped Tungsten Chloride Clusters
the 31P to 35/37Cl direct dipole–dipole interaction has been Experimental Section
3
1
neglected. The P isotropic chemical shift of 349.5 ppm is
not untypical of phosphinidene units.[
6
Syntheses: Reactions between WCl and an approximately threefold
29]
molar excess of elemental red phosphorus were performed in silica
tubes between 200 and 600 °C in intervals of 10 °C. After the com-
positions of the new products were identified by XRD methods,
compositions of the starting materials were adjusted as follows.
Conclusions
6 6
W PCl17: WCl (150 mg, 0.38 mmol; Aldrich, 99.9%) and elemen-
tal red P (15.7 mg, 0.51 mmol; Aldrich, 99%) were mixed under an
argon atmosphere (glovebox), sealed in an evacuated silica tube,
and then heated in a tube furnace for 24 h at 370 °C. The following
reaction is assumed:
The new compounds W PCl and W (PCl)Cl were
6
17
4
10
prepared under moderate heating conditions in order to ap-
proach the mostly unexplored field of missing compounds,
namely the thermally labile cluster compounds. Their struc-
tures comprise phosphido-centered and chlorophosphinid-
6 6 3
18 WCl + 22 P Ǟ 3 W PCl17 + 19 PCl
ene-capped tungsten clusters, as refined from X-ray diffrac- The black microcrystalline powder was removed from the ampoule
3
1
tion data and confirmed by P NMR spectroscopy. The and purified by subliming off the coproduced PCl
3
to give an esti-
compounds appear quite stable in air, showing an un- mated yield (from XRD) of 95% W
6
PCl17
.
changed powder X-ray diffraction pattern after being ex-
posed to air for one week.
The X-ray powder pattern of a single-phase sample was indexed,
and the crystal structure was solved with the program EXPO
[
30]
The dimerization of two W clusters into a W cluster by using direct methods and structure refinements with Winplotr
2
4
has been studied by means of solution chemistry[ and ap- (Fullprof).
32]
[31]
pears to be a nice model for the formation of cluster com-
pounds. Following this model, the combination of two tal red P (15.7 mg, 0.51 mmol; Aldrich, 99%) were mixed under an
W
4
6
PCl11: WCl (150 mg, 0.38 mmol; Aldrich, 99.9%) and elemen-
WϵW dimers leads to the Jahn–Teller distorted tetranu- argon atmosphere (glove box), sealed in an evacuated silica tube,
clear cluster with rectangular- or butterfly-shaped W clus- and then heated in a tube furnace for 24 h at 500 °C. The following
4
reaction is assumed:
ter cores. Both motifs have been reported for Mo X -
4
4
[22]
(
OPr) clusters with X = Cl and Br.
The planar butadi- 12 WCl + 16 P Ǟ 3 W PCl + 13 PCl3
8
6 4 11
ene-type cluster core is also present in W (PCl)Cl . Upon
4
10
The product contained black platelike crystals of W
amounts of needlelike WCl crystals (Ͻ5%) that were located at
one end of the silica tube, and PCl . After PCl was sublimed off,
the product contained an estimated yield (from XRD) of 95%
PCl11. A single crystal of W PCl11 was selected for X-ray struc-
4
PCl11, small
addition of another WϵW dimer to the butterfly-type clus-
ter core, a hexanuclear cluster core is formed, similar to the
one that is present in the structure of W PCl (Figure 7).
4
3
3
6
17
W
4
4
ture refinement.
6 4
The compounds W PCl17 and W (PCl)Cl10 show an unchanged
powder X-ray pattern after exposure to air for one week.
A transition from W PCl17 into W PCl11 occurs with the presence
6
4
of excess elemental phosphorus when heating near or above 380 °C.
The following reaction is assumed:
6
W
6
PCl17 + 4 P Ǟ 9 W
Powder X-ray Diffraction: W
rhombic space group Imm2, a = 6.7835(2) Å, b = 15.8762(3) Å, c
4
PCl11 + PCl
3
–1
6
PCl17, M = 1736.77 gmol , ortho-
r
3
=
10.0727(2) Å, V = 1084.79 Å , F(000) = 1496, ρcalcd. (Z = 2) =
–
3
5.31679 gcm , θ range = 2.5–60°, Cu-Kα1 (λ = 1.54060 Å), T =
293(2) K, 509 measured data (STOE StadIP). Structure solution
by direct methods (EXPO 2009), structure refinement by global
refinement (FullProf Suite), data to parameter ratio: 11.8:1, final
2
R indices: R
p
= 0.0522, Rwp = 0.0693, RBragg = 0.0673, χ = 2.8613.
Figure 7. Fragment condensation scheme arising from two WϵW
dimers forming Jahn–Teller distorted (transition state in parenthe-
ses) tetranuclear clusters with a square-planar or butterfly-type
cluster core. The addition of another WϵW dimer yields the hexa-
Single-Crystal
X-ray
Diffraction:
W
4
(PCl)Cl10
,
M
r
=
–
1
1156.32 gmol , monoclinic space group C2/m, a = 13.257(3) Å, b
3
= 9.850(2) Å, c = 11.400(2) Å, β = 91.38(2)°, V = 1488.2(5) Å ,
F(000) = 1992, ρcalcd. (Z = 4) = 5.161 gcm , μ = 32.863 mm ,
–
3
–1
nuclear cluster core obtained in the structure of W
6
PCl17
.
–
1
approximate crystal dimensions 0.14ϫ0.1ϫ0.04 mm , θ range =
.58–25.97°, Mo-K (λ = 0.71073 Å), T = 293(2) K, 5240 measured
2
α
Although the potential of the new compounds remains
unknown, it has been shown that metal clusters as well as
metal surfaces often reveal common modes of substrate
binding and may provide special properties. This may be
challenging in the case of the chloro-phosphinidene ligand,
data (STOE IPDS) of which 1524 (Rint = 0.1162) unique; Lorentz
and polarization correction (STOE IPDS Software), absorption
correction (X-Red/X-Shape). Structure solution by direct methods
2
(
SHELX-97), full-matrix least-squares refinement on F , data to
parameter ratio: 19.3:1, final R indices: [IϾ2σ(I)]: R1 = 0.0438,
which is situated on rectangular crystal faces of air-stable wR2 = 0.0693, R indices (all data): R1 = 0.0737, wR2 = 0.0773,
2
W (PCl)Cl .
GOOF on F = 0.895.
4
10
Eur. J. Inorg. Chem. 2011, 4063–4068
© 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
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4067

M. Ströbele, K. Eichele, H.-J. Meyer
FULL PAPER
Magnetic Measurements: Magnetic susceptibility measurements
were performed in gelatine capsules with a SQUID magnetometer
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Published Online: May 26, 2011
4068
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Eur. J. Inorg. Chem. 2011, 4063–4068