Diselenolate- and ditellurolate-carborane gold complexes

Article abstract of DOI:10.1039/c3dt50624j

Gold complexes with selenolate and tellurolate carborane ligands [E ₂C₂B₁₀H₁₀]^2- (E = Se, Te) have been synthesized by reaction of a freshly prepared solution of [1,2-(LiE)₂C₂B₁₀H₁₀] (E = Se, Te) with [AuClL] (L = PPh₃, PPh₂Me, PPh₂py) in a 1:2 molar ratio or [Au₂Cl₂(P～P)] [P～P = dppf, 1,1′-bis(diphenylphosphano)ferrocene; dppe, 1,2-bis(diphenylphosphano) ethane; dppc, 1,2-bis(diphenylphosphano)-o-carborane] in a 1:1 molar ratio affording complexes [Au₂(μ-1,2-E₂C₂B ₁₀H₁₀)L₂] or [Au₂(μ-1,2-E ₂C₂B₁₀H₁₀)(P～P)], respectively. The gold(iii) species PPN[Au(E₂C₂B₁₀H ₁₀)₂] (PPN = bis(triphenylphosphano)iminium) have been afforded by reaction of PPN[AuCl₄] with [1,2-(LiE)₂C ₂B₁₀H₁₀]. Complex [Au₄(μ-1,2- Se₂C₂B₁₀H₁₀)₂(μ-dppc) ₂] displays a tetranuclear structure, different from the dinuclear cyclic arrangement proposed for other complexes with diphosphanes of [Au ₂(μ-1,2-Se₂C₂B₁₀H ₁₀)(P～P)] stoichiometry.

Full text of DOI:10.1039/c3dt50624j

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Diselenolate- and ditellurolate-carborane gold
complexes†
Cite this: Dalton Trans., 2013, 42, 10454
Olga Crespo,*a M. Concepción Gimeno,*a Adriana Ilie,a,b Antonio Laguna,a
Isaura Ospinoa and Cristian Silvestrub
2−
Gold complexes with selenolate and tellurolate carborane ligands [E2C2B10H10
]
(E = Se, Te) have been
synthesized by reaction of a freshly prepared solution of [1,2-(LiE)2C2B10H10] (E = Se, Te) with [AuClL] (L =
PPh3, PPh2Me, PPh2py) in a 1 : 2 molar ratio or [Au2Cl2(P∼P)] [P∼P = dppf, 1,1’-bis(diphenylphosphano)-
ferrocene; dppe, 1,2-bis(diphenylphosphano)ethane; dppc, 1,2-bis(diphenylphosphano)-o-carborane] in
a
1 : 1 molar ratio affording complexes [Au2(μ-1,2-E2C2B10H10)L2] or [Au2(μ-1,2-E2C2B10H10)(P∼P)],
Received 6th March 2013,
Accepted 13th May 2013
respectively. The gold(III) species PPN[Au(E2C2B10H10)2] (PPN bis(triphenylphosphano)iminium)
=
have been afforded by reaction of PPN[AuCl4] with [1,2-(LiE)2C2B10H10]. Complex [Au4(μ-1,2-
Se2C2B10H10)2(μ-dppc)2] displays a tetranuclear structure, different from the dinuclear cyclic arrangement
proposed for other complexes with diphosphanes of [Au2(μ-1,2-Se2C2B10H10)(P∼P)] stoichiometry.
DOI: 10.1039/c3dt50624j
www.rsc.org/dalton
design of materials with specific properties which may not be
achieved by the analogous sulfur derivatives.
Introduction
A search in the CCDC leads to about 50 hits for gold(I)1 and
gold(III)2 complexes containing selenolate and tellurolate E2C2B10H10
Coordination chemistry of the dichalcogenolate [1,2-
2−
]
(E = Se, Te) ligands is widely represented.5 The
ligands, from which only 8 contain tellurolate ligands. This crystal structures of lanthanide (Dy Ho)6 and transition metal
result contrasts with more than 1100 hits found for gold thio- complexes of Pt,7 Rh,8 Fe,9 Ir,10 Co11 and Ru8i,12 have been
late derivatives whose X-ray structures have been elucidated. reported. Many of them are mononuclear or polyhomonuclear
Among these 50 examples only the monoselenolate gold derivatives, but heteropolynuclear8g–i,10i,11e,13 complexes are
derivatives [AuL(PPh3)] [L = 1-Se-2-Me-C2B10H10−, 1-Se-C2B10H11
]
also known. These complexes contain closo-carborane cages
and only two examples containing nido-carborane ligands have
−
have been reported1l,s with carborane ligands.
It has been described that gold selenolate complex for- been described.8i,10i No gold complex has been described as
mation in proteins is more easily achieved than the formation far as we know.
of gold thiolate complexes.3 Recently the mode of exchange
Thus in this work we report the synthesis of gold(I) and
reactions at the Au(I) center in gold selenolate in the presence gold(III) complexes with the diselenolate and ditellurolate
or absence of Se⋯N interactions has been reported. Also carborane ligands [1,2-E2C2B10H10]2− (E = Se, Te).
recently the use of selenolate in the synthesis of gold nanoclus-
ters has been described, which exhibit more stability against
degradation in solution than thiolate protected nanoclusters.4
Discussion
Thus, seleno and tellurolate gold chemistry still represents
a hot topic in gold chemistry because it is scarcely represented,
Reaction of [1,2-(LiE)2C2B10H10] (E = Se, Te) with [AuClL] (L =
but also due to different reactivities observed, compared with
the well known thiolate chemistry. This fact may be relevant as
to the dinuclear complexes with tertiary phosphanes of stoichio-
selenolate and tellurolate complexes could be useful for the
PPh3, PPh2Me, PPh2py) in a 1 : 2 molar ratio (Scheme 1) leads
metry [Au2(μ-1,2-Se2C2B10H10)L2] [1, E = Se, L = PPh3; 2, E =
Te, L = PPh3; 3, E = Se, L = PPh2Me; 4, E = Se, L = PPh2py]. The
31P{1H} NMR spectra of these complexes display one resonance
aDepartamento de Química Inorgánica, Instituto de Síntesis Química y Catálisis
at about 36 ppm. The 77Se NMR spectra of 1 and 4 display one
Homogénea (ISQCH), Universidad de Zaragoza-CSIC, E-50009 Zaragoza, Spain.
singlet at about 410 ppm. 77Se NMR chemical shifts for
E-mail: ocrespo@unizar.es
bDepartamentul de Chimie, Centrul de Chimie Supramoleculara Organica si
different selenolate gold derivatives have been reported and
Organometalica (CCSOOM), Facultatea de Chimie si Inginerie Chimica,
revised14 and spread over a wide range. Values observed for
Universitatea Babes-Bolyai, 400028 Cluj-Napoca, Romania
complexes 1 and 4 resemble those observed for complexes [Au-
†CCDC 927127 for complexes 1 and 7. For crystallographic data in CIF or other
electronic format see DOI: 10.1039/c3dt50624j
(SeC2B10H11)L] (L = PPh3, AsPh3) with the monoselenolate
10454 | Dalton Trans., 2013, 42, 10454–10459
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Scheme 1 i = 2 [AuClL] (L = PPh3, PPh2Me, PPh2Py]; ii = [Au2Cl2(dppe)] or [Au2Cl2(dppf )]; iii = [Au2Cl2(dppc)]; iv = 1/2 PPN[AuCl4].
Fig. 1 (a) Molecular diagram of complex [Au2(μ-1,2-Se2C2B10H10)(PPh3)2] (1). (b) Molecular diagram of complex [Au2(μ-1,2-Se2C2B10H10)(PPh2Me)2] (3). Radii are
arbitrary. Hydrogen atoms have been omitted for clarity.
carborane ligand1s and lie in the lower field region reported stoichiometry [Au2Cl2(P∼P)] [P∼P = dppf, 1,1′-bis(diphenyl-
for gold(I) complexes and resemble that observed for phosphano)ferrocene; dppe, 1,2-bis(diphenylphosphano)-
[Au2{SeC6H4(2-CH2NMe2)}2(μ-dppf)] at 424.2 ppm in which ethane; dppc, 1,2-bis(diphenylphosphano)-o-carborane] in
electronic delocalization through the ferrocene unit is a 1 : 1 molar ratio it is possible to isolate and characterize
possible, whereas the resonances corresponding to similar complexes [Au2(μ-1,2-Se2C2B10H10)(μ-dppf)] (5), [Au2(μ-1,2-
complexes [Au2{SeC6H4(2-CH2NMe2)}2(μ-P∼P)] with other Te2C2B10H10)(μ-dppe)] (6) and [Au4(1,2-Se2C2B10H10)2(dppc)2]
diphosphanes such as dppm or dppe appear at 161.3 and (7) (Scheme 1). In the rest of the cases the reactions lead to a
125.2, respectively.1c Crystal structures of complexes 1 and 3 mixture of different products which include the expected ones.
have been elucidated (Fig. 1). For both complexes the proposed The 31P{1H} NMR resonances in the spectra of 5 and 6 and
stoichiometry was confirmed, although for 1 [crystal system, the 77Se NMR resonance in the spectra of 5 appear at similar
monoclinic; space group, P21/n; cell: a, 10.505(2); b, 18.638(4); fields as those observed for the complexes with monophos-
c, 23.597(5); α, 90; β, 100.75(3); γ, 90] the quality of the data phanes described previously, except for complex 7, which dis-
was not good and for compound 3 [crystal system, triclinic; plays a singlet in its 31P{1H} NMR spectrum at 54.8 ppm. We
ˉ
space group, P(1); cell: a, 11.556(2); b, 12.689(3); c, 13.087(3); α, propose for 5 and 6 similar structures to those obtained
80.66(3); β, 88.96(3); γ, 75.74(3)] data collection was not com- for similar complexes containing the carborane dithiolate
2− 15
plete. Thus, no comparison of bond distances and angles with [S2C2B10H10
]
.
They consist of dinuclear units in which
other complexes can be made, although a molecular diagram the two gold centers are bridged by a dichalcogenide and a
is shown in Fig. 1.
diphosphane ligand.
From the reaction of [1,2-(LiE)2C2B10H10] (E = Se, Te) with
A different structure has been confirmed for 7 through
dinuclear gold complexes with bridging diphosphanes of X-ray studies. Compound 7 is a tetranuclear complex (Fig. 2) in
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Fig. 3 Molecular diagram of one of the anions of [Au(1,2-Se2C2B10H10)2]− in
complex 8. Radii are arbitrary. Hydrogen atoms have been omitted for clarity.
atom compared with the sulfur one, the rigidity of the carbor-
ane ligands and the trend of the diphosphane to act in a
chelate mode lead to a tetranuclear structure.
Fig. 2 Molecular diagram of complex [Au4(1,2-Se2C2B10H10)2(dppc)2] (7). Radii
are arbitrary. Hydrogen atoms have been omitted for clarity.
Reaction of [1,2-(LiE)2C2B10H10] (E = Se, Te) with PPN-
[AuCl4] leads to complexes PPN[Au(1,2-E2C2B10H10)2] E =
[Se (8), Te (9)]. The resonance of compound 8 in the 77Se NMR
spectrum appears at 739.5 ppm, this resonance appears at a
much lower field than in the gold(I) complexes described
above. The resonance in 8 appears also at a lower field than
that reported for other gold(III) derivatives14 such as [AuCl3-
Table 1 Bond distances (Å) and angles (°) for gold complexes with carborane
selenolate ligands
[AuL1(PPh3)]1l
[AuL2(PPh3)]1s
[Au4(L3)2(L4)2] (7)
Au⋯Au
Aua–Se
3.3035(4)c
2.4167(4)
3.2384(9)d
2.4094(8)
2.3954(10)
2.6132(15)
2.6905(7)
(SePh2)] (534.7 ppm)17 or NBu4[Au(Se∼Se)2] [Se∼Se
=
2.4254(6)
3.4783(6)c
Aub–Se
1,3-dithiole-2-selenone-4,5-diselenolate (686.7 ppm) and
1,3-dithiole-2-thione-4,5-diselenolate (693.1 ppm)].
X-ray studies confirm the structure proposed for complex 8
(Fig. 3), in which the gold centre displays a square planar geo-
metry, although not all the data were collected. Compound 8
Aua–P
Aub–P
2.2740(13)
1.955(5)
2.2690(10)
1.940(4)
2.4075(14)
2.3208(9)
1.938(3)
1.937(3)
1.690(4)
C–Se
ˉ
crystallizes in the triclinic system, space group P(1). Cell con-
C–Ce
1.703(7)
174.82(7)
1.682(6)
175.08(3)
P–Aua–Se
Se–Aua–Se
P–Aub–P
Se–Aub–Se
stants, 13.719(3); b, 14.053(3); c, 15.058(3), α, 90.46(3), β,
109.19(3), γ, 107.85(3). This compound represents one of the few
diselenolate gold(III) complexes structurally characterized.18,2b
169.692(12)
95.23(5)
86.46(3)
a Di-coordinated
environment.
b Tetrahedral
environment.
c Intermolecular. d Intramolecular. e In the carborane diselenolate. L1 =
[1-Se-2-Me-C2B10H10]−. L2 = [1-Se-C2B10H11]−. L3 = [1,2-Se2C2B10H10
] .
2−
L4 = 1,2-(PPh2)2C2B10H10
.
Conclusions
Gold(I) and gold(III) complexes with the dichalcogenolate
2−
carborane ligands [E2C2B10H10
]
(E = Se, Te) have been
which two gold centers are coordinated to two selenium atoms
synthesized from the reaction of [1,2-(LiE)2C2B10H10] with the
of different diselenolate ligands and display linear distorted corresponding gold-chloride derivative. They contribute to the
linear coordination [Se–Au–Se = 169.692(13)°] (Table 1). The few examples of gold selenolates and tellurolates reported in
structure is similar to that observed for the analogous sulfur
the literature, compared with disulfide complexes and are the
first gold complexes with these dichalcogenolate ligands. For
derivative [Au4(μ-1,2-S2C2B10H10)2(μ-dppc)2].16
The Au⋯Au distance between these gold atoms is 3.2385(9) complexes [Au2(μ-1,2-Se2C2B10H10)(P∼P)] a cyclic structure is
Å. The Au–P and Au–Se bond distances resemble those
proposed, in which the diselenolate and the diphosphane act
described for the complexes with carborane monoselenolate in a bridging mode. When the diphosphane is dppc the X-ray
ligands [Au(1-SeC2B10H11)(PPh3)] and [Au(2-Me,1-SeC2B10H11)- study confirms the formation of a tetranuclear derivative of
(PPh3)]. The other two gold centers display a tetrahedral
stoichiometry [Au4(μ-1,2-S2C2B10H10)2(μ-dppc)2] (7) in which
environment. They are coordinated to diphosphane and disele- two gold centers are coordinated to two selenide atoms of
nolate carborane ligands which act in a chelate mode. The different diselenolate ligands and display distorted linear
Se–Au–Se and P–Au–P angles are 95.18(5)° and 86.43(3)°,
coordination and the other two gold centers display tetra-
respectively. The dihedral angle between planes defined by hedral geometry. The bulky and rigid nature of the carborane
Se/Au/Se and P/Au/P is 92.3°. The Au–Se distances of about cluster of the diphosphane could be responsible for the
2.6 Å are longer than those observed for the gold atoms in a
formation of a different structure from that proposed for
linear environment. Despite the bigger size of the selenium the complexes with other diphosphanes.
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36.8 (s). 77Se NMR (CDCl3, ppm): 416.5 (s). IR (cm−1): ν(BH) =
2592 (st).
[Au2(μ-1,2-E2C2B10H10)(μ-P∼P)][P∼P = dppf, E = Se (5);
Experimental
General comments
Infrared spectra were recorded in the range 4000–200 cm−1 on P∼P = dppe E = Te (6)]. The procedure used to synthesize
a Perkin-Elmer 883 spectrophotometer using ATR accessory. complexes 5 and 6 was similar to that described for com-
C, H, N and S analyses were carried out with a Perkin-Elmer pounds 1–4 from [Au2Cl2(µ-P∼P)] [0.25 mmol: 254 mg, µ-P∼P =
240B or 2400 microanalyzer. NMR spectra were recorded on dppf E = Se (5); 215 mg, µ-P∼P = dppe, E = Te (6)] and
a Varian Unity 300, a Bruker ARX 300 and a Bruker ARX-400 [(LiE)2(C2B10H10)] (0.2 mmol) in diethyl ether under an argon
spectrometer in CDCl3. The ARX-400 MHz spectrometer was atmosphere. The product was obtained by addition of
used in almost all the cases, when an ARX 300 MHz spectro- n-hexane. 5: Yield 55%, pale yellow colour. Analytical data (%);
meter is used it has been specified. Chemical shifts are found: C, 32.83; H, 2.11; calculated for C46H50Au2B10Fe2P2Se2:
reported relative to SiMe4 (1H and 13C), CFCl3 (19F), 85% C, 33.16; H, 2.53. 1H NMR (CDCl3, ppm): 0–3.5 (m, br, 10H,
H3PO4 (31P) and Me2Se (77Se) as external standards.
BH), 4.10–4.23 (m, br, 4H, CH), 4.40–4.53 (m, br, 4H, CH),
7.40–7.62 (v.m, br, 20H, Ph). 31P{1H} NMR (CDCl3, ppm) 36.1
(s). 77Se NMR (CDCl3, ppm) 408.3 (s). IR (cm−1): ν(BH) = 2565
Synthesis
The carborane [1,2-(LiE)2C2B10H10] species were prepared and (st). 6: Yield 51%, pale yellow colour. Analytical data (%),
used “in situ” according to literature methods.8b The gold found: C, 27.83; H, 2.01; calculated for C28H34Au2B10P2Te2:
starting materials [AuClL] [L = PPh3, PPh2Me, PPh2py],19 C: 28.26; H. 2.88. 1H NMR (CDCl3, ppm): 0–3 (m, br, 10H, BH),
[Au2Cl2(P∼P)] [P∼P
[AuCl4]23 were prepared according to published procedures. (CDCl3, ppm) 35.0 (s). IR (cm−1): ν(BH) = 2546 (st).
Reaction solvents were of reagent grade and were distilled [Au4{1,2-(PPh2)2C2B10H10}2{μ-1,2-Se2C2B10H10}2] (7). The
=
dppf,20 dppe,21 dppc22] and PPN- 2.72 (br, 4H, CH), 7.44–7.65 (v.m, br, 20H, Ph). 31P{1H} NMR
from the appropriate drying agents under argon prior to use, compound was synthesized through a similar procedure to
when required or obtained from the system purification that described previously from [Au2Cl2(dppc)] (0.25 mmol,
solvent (SPS) PS-MD-5 Innovative technology, Scharlab.
243 mg) and [(LiE)2(C2B10H10)] (0.2 mmol) in diethyl ether
[Au2(1,2-E2C2B10H10)(PPh2R)2][R = Ph, E = Se (1), Te (2); R = under a nitrogen atmosphere. The product, as a pale yellow
Me, E = Se (3); R = Py, E = Se (4)]. [AuCl(PPh2R)] (0.45 mmol: solid, was obtained by addition of n-hexane. Yield 72%.
222 mg R = Ph; 200 mg R = Me; 223 mg R = Py) was added, Analytical data (%), found: C, 28.17; H, 3.49; calculated for
1
under an argon atmosphere, to a round bottom flask contain- C56H80Au4B40P4Se4: C, 27.87; H, 3.34. H NMR (CDCl3, ppm):
ing a diethyl ether solution of [(LiE)2(C2B10H10)] [25 mL, 0.5–3 (m, br, 40H, BH), 7.44–7.55 (m, br, 20H, Ph), 7.83–8.06
0.2 mmol; prepared from LinBu (0.4 mmol, 250.0 μL) (1.6 M in (m, br, 20H, Ph). 31P{1H} NMR (CDCl3, ppm) 54.8 (s). IR
hexane), ortho-carborane (28.8 mg, 0.2 mmol) and Se (cm−1): ν(BH) = 2556 (st).
(0.4 mmol, 31.5 mg) or Te (0.4 mmol, 51.04 mg]. The mixture
PPN[Au(1,2-E2C2B10H10)2][E = Se (8), Te (9)]. The compound
was stirred for 3.5 h. The resulting solution was concentrated was synthesized through a similar procedure to that described
to dryness under reduced pressure. The residue was extracted previously from PPN[AuCl4] (0.15 mmol, 131 mg) and
with dichloromethane and filtered over celite. Concentration [(LiE)2(C2B10H10)] (0.2 mmol) in diethyl ether under a nitrogen
to ca. 3 mL and addition of n-hexane lead to complexes 1–4. 1: atmosphere. The products were obtained by addition of
Yield 67%, pale yellow colour. Analytical data (%), found: C, n-hexane. 8: Yield 62%, red colour. Analytical data (%), found:
37.16; H, 3.18; calculated for C38H40Au2B10P2Se2: C, 37.45; H, C, 35.60; H, 4.02; N, 1.07; calculated for C40H50AuB20NP2Se4:
1
1
3.31. H NMR (CDCl3, ppm): 1–3.5 (m, br, 10H, BH), 7.40–7.67 C, 35.96; H, 3.77; N, 1.04. H NMR (CDCl3, ppm): 0–3 (m, br,
(br, 30H, Ph). 31P{1H} NMR (CDCl3, ppm) 36.3 (s). 77Se NMR 20H, BH), 7.43–7.51 (m, br, 15H, Ph), 7.66–7.70 (m, br, 15H,
(CDCl3, ppm): 412.4 (s). IR (cm−1): ν(BH) = 2563 (st). 2: Yield Ph). 31P{1H} NMR (CDCl3, ppm) 21.2 (s). 77Se NMR (CDCl3,
57%, green colour. Analytical data (%), found: C, 35.13; H, ppm): 739.5 (s). IR (cm−1): ν(BH) = 2564 (st). 9: Yield 42%,
3.04; calculated for C38H40Au2B10P2Te2: C, 34.68; H, 3.06. yellow colour. Analytical data (%), found: C, 32.08; H, 3.28; N,
1H NMR (CDCl3, ppm): 1–3 (m, br, 10H, BH); 7.00–7.50 (m, 1.3; calculated for C40H50AuB20NP2Te4: C, 31.39; H, 3.29; N,
1
br, 30H, Ph). 31P{1H} NMR (CDCl3, ppm) 36.4 (s). IR (cm−1): 0.91. H NMR (CDCl3, ppm): 0–3 (m, br, 20H, BH), 7.45–7.50
ν(BH) = 2584 (st). 3: Yield 50%, pale yellow colour. Analytical (m, br, 20H, Ph), 7.66–7.68 (m, br, 10 H, Ph). 31P{1H} NMR
data (%), found: C, 31.20; H, 3.78; calculated for (CDCl3, ppm) 21.3 (s). IR (cm−1): ν(BH) = 2563 (st).
1
C28H36Au2B10P2Se2: C, 30.72; H, 3.31. H NMR (CDCl3, ppm):
1–3 (m, br, 10H, BH), 1.88 (d, 6H, Me, J(P–H) = 9.6 Hz),
Crystallography
7.36–7.48 (br, 20H, Ph). 31P{1H} NMR (CDCl3, ppm) 21.4 (s). IR All crystals were mounted in inert oil on a glass fiber and
(cm−1): ν(BH) = 2573 (st). 4: Yield 60%, pale yellow colour. transferred to the cold gas stream of an Xcalibur Oxford Diffr-
Analytical data (%), found: C, 34.93; H, 3.37; N, 2.10; calcu- action diffractometer equipped with a low-temperature attach-
lated for C36H38Au2B10N2P2Se2: C, 35.42; H, 3.13; N, 2.29. ment. Data were collected using monochromated Mo Kα
1H NMR (CDCl3, ppm): 0–3.5 (m, br, 10H, BH), 7.28–7.40 (v.m, radiation (λ = 0.71073 Å). Scan type ω. Absorption correction
br, 10H, Ph), 7.54–7.60 (v.m, br, 10H, Ph), 7.83–7.87 (v.m, br, based on multiple scans was applied with the program
4H, Ph), 8.62–8.63 (m, br, 4H, Ph). 31P{1H} NMR (CDCl3, ppm) SCALE3 ABSPACK.24 The structures were refined on F2 using
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281–289; (v) D. Naumann, W. Tyrra, S. Quadt, S. Buslei,
I. Pantenburg and M. Schafer, Z. Anorg. Allg. Chem., 2005,
631, 2733–2737; (w) E. S. Lang, C. Maichle-Mossmer and
J. Strahle, Z. Anorg. Allg. Chem., 1994, 620, 1678–1685;
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Table 2 X-ray data for complex 7
Compound
7
Formula
T/K
Crystal system
Space group
a (Å)
b (Å)
c (Å)
C
60H88Au4B40Cl8P4Se4
173(2)
Triclinic
P1
ˉ
11.550(2)
15.209(3)
16.081(3)
105.15(3)
110.39(3)
106.59(3)
2323.9(14)/1
1.967
8.198
1296
50
32 431/8144
0.0189
0.5600, 0.1514
24/541
0.0181
0.0435
α (°)
β (°)
γ (°)
V (Å3)/Z
DX (Mg m−3
)
μ (mm−1
F(000)
2θmax
)
Refl.: measured/independent
R(int)
Transmissions
Restraints/parameters
R(I > 2σ(I))
wR(F2, all Refl.)
S
1.031
1.171
Max. Δρ (e Å−3
)
the program SHELXL-97.25 All non-hydrogen atoms were
refined anisotropically. Hydrogen atoms were included using a
riding model. Further details of the data collection and refine-
ment are given in Table 2.
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Acknowledgements
We thank the Ministerio de Economía y Competitividad-
FEDER (No. CTQ2010-20500-C02-01) and DGA-FSE (E77).
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Dalton Trans., 2013, 42, 10454–10459 | 10459