Crystal Structures of Hydrazinium(II) Salts of [SbF6]- and [Sb2F11]-

Article abstract of DOI:10.1002/zaac.201500110

N₂H₆(Sb₂F₁₁)₂ was synthesized by the reaction of N₂H₆F₂ with excess of SbF₅ in anhydrous hydrogen fluoride (aHF). It crystallizes in the triclinic space group P 1ˉ (No. 2) with a = 6.6467(3) ?, b = 8.3039(4) ?, c = 8.3600(5) ?, α = 76.394(5) ^o, β = 70.161(5) ^o, γ = 70.797(5) ^o, V = 405.90(4) ?³ at 150 K, Z = 2. When it is redissolved in aHF, it solvolysis with the release of SbF₅ yielding N₂H₆(SbF₆)₂ which crystallizes in the monoclinic C2/c space group (No. 15) with a = 7.3805(3) ?, b = 12.3248(5) ?, c = 10.4992(4) ?, β = 92.218(4) ^o, V = 954.33(7) ?³ at 150 K, and Z = 8. No other phases were observed in crystallization products when different molar ratios of N₂H₆F₂/SbF₅ (1:1,2:3,1:3) in aHF were used as starting materials.

Full text of DOI:10.1002/zaac.201500110

Journal of Inorganic and General Chemistry
www.zaac.wiley-vch.de
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
DOI: 10.1002/zaac.201500110
Crystal Structures of Hydrazinium(II) Salts of [SbF6]– and [Sb2F11]–
Zoran Mazej*[a] and Evgeny A. Goreshnik[a]
Dedicated to Dr. Karel Lutar (the Ph.D. Thesis Tutor of Z.M) who did Preliminary Experiments in 1992 and
Deceased in 2000
Keywords: Hydrazinium ions; Antimony; Fluorides; Crystal structure
Abstract. N2H6(Sb2F11)2 was synthesized by the reaction of N2H6F2 which crystallizes in the monoclinic C2/c space group (No. 15) with
with excess of SbF5 in anhydrous hydrogen fluoride (aHF). It crys-
a = 7.3805(3) Å, b = 12.3248(5) Å, c = 10.4992(4) Å, β = 92.218(4)
o, V = 954.33(7) Å3 at 150 K, and Z = 8. No other phases were ob-
served in crystallization products when different molar ratios of
N2H6F2/SbF5 (1:1,2:3,1:3) in aHF were used as starting materials.
¯
tallizes in the triclinic space group P1 (No. 2) with a = 6.6467(3) Å,
o
o
b = 8.3039(4) Å, c = 8.3600(5) Å, α = 76.394(5) , β = 70.161(5) , γ
= 70.797(5) o, V = 405.90(4) Å3 at 150 K, Z = 2. When it is redissolved
in aHF, it solvolysis with the release of SbF5 yielding N2H6(SbF6)2
small amount of N2H6(SbF6)2. In previous report only
N2H6(SbF6)2 has been detected as the final product.[1] The
reason is most likely in different concentrations of SbF5 in
aHF. When redissolved, N2H6(Sb2F11)2 solvolysis in aHF
[Equation (2)]:
1 Introduction
The synthesis of hydrazinium(II) hexafluoridoantimonate,
N2H6(SbF6)2 was first time reported in 1990.[1] It was charac-
terized by chemical analysis and vibrational spectroscopy. Its
thermal decomposition was also studied. In the same paper it
was given that its X-ray powder diffraction pattern (measured
at ambient temperature) can be indexed on the basis of a mo-
noclinic cell with a = 8.22(2) Å, b = 10.04 Å, c = 9.51 Å, β =
97.2(2) o and V = 780 Å3. Since no other structure information
have been reported, we decided to reinvestigate its synthesis
and try to prepare single crystals of N2H6(SbF6)2.
aHF
N2H6(Sb2F11)2 –––Ǟ N2H6(SbF6)2 + 2SbF5
(2)
298 K
Redissolving of dry solid Sb2F11 salts with the use of aHF
is an effective way to eliminate SbF5 from Sb2F11.,[2,3] Both
colorless compounds decompose when they are exposed to air
due to the reaction with moisture.
In this paper, syntheses and crystallizations in the system
N2H6F2 / SbF5 were carried out in anhydrous hydrogen fluor-
ide (aHF) and have yielded two hydrazinium(II) salts contain-
ing the [SbF6]– and [Sb2F11]– anions. N2H6(SbF6)2 and
N2H6(Sb2F11)2 were isolated and their crystal structures were
determined and are described in this paper.
2.2 Crystal Structures of N2H6(SbF6)2 and N2H6(Sb2F11)2
The crystal structures of hydrazinium [N2H6]2+ salts with
fluoridometallate anions are limited to metals (M) in the oxid-
ation states M2 = Be,[4] Sn;[5] M+3 = B,[6] Ga,[7] In,[8] As,[9]
Sb;[10] and M+4 = Ti,[11,12] Zr,[13,14] Si,[15] Ge,[16] Sn.[17] Al-
though N2H6(MVF6)2 (M = P, As, Sb) are known,[1] no data
about their or crystal structures of other N2H6(MVF6)2 (M =
M5+] compounds have been reported so far.
2 Results and Discussion
The crystal data and refinement results of N2H6(SbF6)2 and
N2H6(Sb2F11)2 are summarized in Table 1. Selected bond
length and angles are given in Table 2.
2.1 Syntheses
N2H6(Sb2F11)2 can be prepared by reaction of N2H2F2 with
SbF5 in anhydrous hydrogen fluoride (aHF) [Equation (1)]:
The crystal structure of N2H6(SbF6)2 consists of [N2H6]2+
cations and [SbF6]– anions held together by hydrogen bonds
(Figure 1). The N–N distance determined at 150 K is
1.457(8) Å and it is longer than usually observed.[4,6,13,15,16] It
is comparable to N–N bond lengths found in (N2H6)2F2(SnF6)
(at 123 K: 1.46(3) Å – eclipsed conformation of N2H6)[17] and
N2H6TiF6 (at room temperature: 1.474(7) Å – staggered con-
formation of N2H6).[12]
aHF
N2H2F2 + 4SbF5 –––Ǟ N2H6(Sb2F11)2
(1)
298 K
Although the starting molar ratio n(SbF5)/n(N2H6F2) was
higher than four, the final product was still contaminated with
* Dr. Z. Mazej
E-Mail: zoran.mazej@ijs.si
[a] Jozˇef Stefan Institute
Jamova 39
The symmetry constraints of the space group C2/c require
that the hydrogen atoms of the N2H6 group are in eclipsed (cis)
1000 Ljubljana, Slovenia
Z. Anorg. Allg. Chem. 2015, 641, (7), 1216–1219
1216
© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Journal of Inorganic and General Chemistry
www.zaac.wiley-vch.de
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
Table 1. Summary of crystal data and refinement results for
N2H6(SbF6)2 and N2H6(Sb2F11)2.
N2H6(SbF6)2
150
N2H6(Sb2F11)2
T /K
150
Crystal system
a /Å
b /Å
c /Å
monoclinic
7.3805(3)
12.3248(5)
10.4992(4)
/
triclinic
6.6467(3)
8.3039(4)
8.3600(5)
76.394
α /°
β /°
92.218(4)
/
954.33(7)
C2/c
70.161(5)
70.797(5)
405.90(4)
P1
2
3.8413
0.71073
6.813
1.029
0.028
0.082
γ /°
V /Å3
¯
Space group
Z
8
Dcalcd. /g·cm–3
λ /Å
3.5184
0.71073
5.826
1.048
0.028
μ /mm–1
GOF indicatora)
b)
R1
c)
wR2
0.070
Figure 1. Packing of [N2H6]2+ cations and [SbF6]– anions in the crystal
structure of N2H6(SbF6)2.
2
2 2
a) GOF = [Σw(Fo –Fc ) /(No–Np)]1/2, where No = no. of reflns and
Np = no. of refined parameters. b) R1 = Σ||Fo|–|Fc||/Σ|Fo|. c) wR2
[Σw(Fo –Fc ) /Σ(w(Fo ) ]
=
2
2 2
2 2 1/2
.
Table 2. Selected distances /Å and angles /° in the crystal structures
of N2H6(SbF6)2 and N2H6(Sb2F11)2.
N2H6(SbF6)2
N2H6(Sb2F11)2
N–N
1.457(8)
2ϫ1.869(3)
2ϫ1.885(3)
2ϫ1.887(3)
/
/
/
2ϫ1.873(3)
2ϫ1.875(3)
2ϫ1.879(3)
/
/
/
/
/
1.439(8)
1.827(2)
1.851(2)
1.873(3)
1.876(2)
1.881(2)
2.011(2)
/
Sb1–F1
Sb1–F2
Sb1–F3
Sb1–F4
Sb1–F5
Sb1–F11
Sb2–F4
Sb2–F5
Sb2–F6
Sb2–F7
Sb2–F8
Sb2–F9
Sb2–F10
Sb2–F11
/
1.843(3)
1.857(3)
1.861(3)
1.867(2)
1.878(2)
2.036(2)
Sb2F11 angles
Sb1–Fb–Sb2a)
Torsion angleb)
/
/
170.74(14)
≈ 7
Figure 2. Part of the crystal structure of N2H6(SbF6)2 showing only
moderate strong hydrogen bonds (dashed lines) between [N2H6]+ and
[SbF6]– ions; thermal ellipsoids are drawn at the 50% probability level.
Symmetry codes: (i) –x, 1–y, 1–z; (ii) 1–x, 1–y, 1–z; (iii) 0.5+x, 0.5+y,
z; (iv) 1+x, y, z; (v) 0.5+x, 0.5+y, z; (vi) 0.5–x, 0.5+y, 0.5–z; (vii) 1–x,
y, 0.5–z; (viii) –x, y, 0.5–z; (ix) x, 1–y, –0.5+z.
a) Bending of two SbF5 groups about Fb (bridging fluorine), which is
expressed in terms of the bridge angle α. b) Torsion of two planar
SbF4,eq groups from eclipsed to staggered conformation expressed in
the torsion angle (ψ).[2,18]
position (Figure 2). There is a twofold axis going through the 3.2 Å and N–H···F Ͼ 130° for moderate (mainly electrostatic)
center of N–N bond. Such eclipsed conformation is rare and it hydrogen bonds,[19] then each [N2H6]2+ cation is involved in
has been observed previously in (N2H6)2F2(SnF6)[17] and moderate hydrogen bonding with six SbF6 units, i.e. each
(N2H6)2F2(TiF6).[11]
hydrogen atom of the NH3 group forms one single contact with
Although hydrogen bonds exists with a continuum of different SbF6 unit (Figure 2).
strengths, it is useful for practical reasons to use classification
There are two crystallographic unique SbF6 units. All six
such as strong, moderate and weak hydrogen bonds.[19] There fluorine atoms of Sb(1)F6 participate in moderate strong
are no strong (quasi-covalent nature) hydrogen bonds with hydrogen. Comparison of Sb–F distances (Table 2) shows that
short F···N = 2.2–2.5 Å contacts[19] present in the crystal struc- both SbF6 octahedra are quite regular, indicating that in ad-
ture. On the basis of proposed model for hydrogen atoms, con- dition to previously mentioned moderate hydrogen bonds there
sidering the packing of the [N2H6]2+ and [SbF6]– ions and are a lot of weak (electrostatic/dispersion)[19] hydrogen bond-
using the proposed parameters H···F = 1.5–2.2 Å, N···F = 2.5– ing interactions.
Z. Anorg. Allg. Chem. 2015, 1216–1219
1217
© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Journal of Inorganic and General Chemistry
www.zaac.wiley-vch.de
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
The crystal structure of N2H6(Sb2F11)2 is composed of
With almost linear dihedral angle (approx. 171°) and very
[N2H6]2+ cations and [Sb2F11]– groups (Figure 3). The exam- small torsion angle (7°, Table 2) the [Sb2F11]– anion (Figure 4)
ples of compounds where the charge of double charged cation is very closed to ideal D4h symmetry.[25]
is compensated by two single charged [Sb2F11]– anions are not
very common. No M(Sb2F11)2 compounds with simple M2+
cations (M2+ = Sn, Pb, transition or alkaline earth metal) have
3 Conclusions
been reported so far.[20,21] The reason must be in unfavorable
packing of small metal M2+ cations and large [Sb2F11]– anions.
Only compounds with complex double charged cations, as for
example [AuXeF4]2+,[22] [Se2I4]2+,[23] and [M(CO)n]2+ (M =
Hg, Pd, Pt, Fe, Ru, Os; n = 2–6),[24] are known.
The single crystals of only two phases, i.e. N2H6(SbF6)2 and
N2H6(Sb2F11)2, were grown in the N2H6F2/SbF5/aHF system
and their crystal structures were determined. The unit cell of
the crystal structure of N2H6(SbF6)2, determined on a single
crystal at 150 K, is in disagreement with previously reported
one indexed on the basis of X-ray powder diffraction (XPD)
photograph obtained at ambient temperature. There could be
two reasons. First, that the indexation gave wrong result due
to the poor quality of obtained XPD photograph or that there
is phase transition resulting in high- and low-temperature
modifications of N2H6(SbF6)2. Unfortunately, single crystals
of N2H6(SbF6)2 were too small to be filled in quartz capillaries
and measured at ambient temperature.
4 Experimental Section
4.1 Apparatus, Techniques and Reagents
Volatile materials (anhydrous HF, F2, SbF5) were handled in a nickel
vacuum line and an all PTFE vacuum system equipped with PTFE
valves as described previously.[26] The nonvolatile materials were ma-
nipulated in a dry box (M. Braun, Germany). The residual water in the
atmosphere within the dry-box never exceeded 1 ppm. The reactions
were carried out in FEP (tetrafluoroethylene-hexafluoropropylene;
Polytetra GmbH, Germany) reaction vessels (height 250–300 mm with
inner diameter 15.5 mm and outer diameter 18.75 mm) equipped with
PTFE valves [27] and PTFE coated stirring bars. Prior to their use all
reaction vessels were passivated with elemental fluorine (Solvay Fluor
and Derivate GmbH, Germany).
Figure 3. Packing of [N2H6]2+ cations and [Sb2F11]– anions in the
crystal structure of N2H6(Sb2F11)2.
The N–N bond length in N2H6 unit equals 1.439(8) Å and
is slightly shorter than in SbF6 salt. In N2H6(Sb2F11)2 the
hydrogen atoms of N2H6 group are in usual staggered (trans)
position. If the same approach is used as for N2H6(SbF6)2 com-
pound, then each [N2H6]2+ cation is involved in six moderate
strong hydrogen bonds with two Sb2F11 units (Figure 4). Sim-
ilar as before, a large number of weak hydrogen bonding con-
tacts are present.
N2H6F2 and SbF3 (Alfa Aesar, 99%) were used as supplied. SbF5 was
prepared in a similar way as reported for AsF5,[28] i.e. by static fluorin-
ation of SbF3 with elemental fluorine in a nickel autoclave at 110 °C.
Higher temperature should be avoided since otherwise SbF5 further
reacts with reaction vessel’s walls forming Ni(SbF6)2. Anhydrous HF
(Linde, Fluorwasserstoff 3.5) was treated with K2NiF6 (Ozark-Mahon-
ing, 99%) for several hours prior to use.
X-ray powder diffraction photographs were obtained using the Debye-
Scherrer technique with Ni-filtered Cu-Kα radiation. Samples were
loaded into quartz capillaries (0.3 mm) in a dry-box. Intensities were
estimated visually. Hydrazine was determined potentiometrically.[29]
4.2 Synthesis of N2H6(Sb2F11)2 and N2H6(SbF6)2
N2H6F2 (0.502 g, 6.98 mmol) was loaded in a reaction vessel in a
glove-box. SbF5 (7.10 g, 32.8 mmol) and anhydrous hydrogen fluoride
(4 mL, aHF) were condensed onto the N2H6F2 and the reaction vessel
was brought to room temperature. Immediately, a clear colorless solu-
tion was obtained. The volatiles were slowly pumped off at room tem-
perature, leaving behind colorless solid. The final mass of the isolated
solid was 6.335 g [calcd. for N2H6(Sb2F11)2: 6.553 g] corresponding
to the molar ration N2H6F2:SbF5 = 1:3.85 on the basis of starting
amount of N2H6F2. Chemical analysis of N2H4 in N2H6F2·3.85SbF5:
calcd. 3.52 wt%; found 3.5 wt%. X-ray powder diffractions data show
only the presence of N2H6(Sb2F11)2.
Figure 4. Part of the crystal structure of N2H6(Sb2F11)2 showing only
moderate strong hydrogen bonds (dashed lines) between [N2H6]2+ and
[Sb2F11]– ions; thermal ellipsoids are drawn at the 50% probability
level. Symmetry codes: (i) 1+x, y, z; (ii) 1–x, 2–y, 1–z; (iii) 2–x, 2–y,
1–z.
Z. Anorg. Allg. Chem. 2015, 1216–1219
1218
© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Journal of Inorganic and General Chemistry
www.zaac.wiley-vch.de
ARTICLE
Zeitschrift für anorganische und allgemeine Chemie
A large amount of aHF (8 mL) was condensed onto N2H6(Sb2F11)2
(200 mg). Volatiles were pumped away and fresh aHF was added. This
was repeated three times. The measured X-ray powder difraction data
of the bulk material and of the simulated one from single crystal deter-
mination of N2H6(SbF6)2 were essentially identical.
References
[1] D. Gantar, A. Rahten, J. Therm. Analysis 1990, 36, 553–558.
[2] Z. Mazej, P. Benkicˇ, Inorg. Chem. 2003, 42, 8337–8343.
[3] E. Bernhardt, B. Bley, B. R. Wartchow, H. Willner, E. Bill, P.
Kuhn, I. H. T. Sham, M. Bodenbinder, R. Bröchler, F. Aubke, J.
Am. Chem. Soc. 1999, 121, 7188–7200.
[4] M. R. Anderson, S. Vilminot, I. D. Brown, Acta Crystallogr., Sect.
B 1973, 29, 2961–2962.
[5] V. Kaucˇicˇ, I. Leban, S. Gasˇpericˇ-Skander, D. Gantar, A. Rahten,
4.3 Crystal Growth of N2H6(Sb2F11)2 and N2H6(SbF6)2
ˇ
A T-shaped apparatus consisting of two FEP tubes (6 mm and 19 mm
outer diameter) was used for single crystal growth. The product of
reaction between N2H6F2 and SbF5 corresponding to molar ration
N2H6F2:SbF5 = 1:3.85 was loaded (approximately 150 mg) into the
wider arm of the crystallization vessel in a dry-box. Afterwards aHF
(4 mL) was condensed onto the starting material at 77 K. The crystalli-
zation mixture was brought up to ambient temperature and the clear
solution, which had developed, was decanted into the narrower arm.
The evaporation of the solvent from this solution was carried out by
maintaining a temperature gradient corresponding to about 10 K be-
tween both tubes for 2 months. The effect of this treatment was to
enable aHF to be slowly evaporated from the narrower into the wider
tube leaving the crystals. Two different types of crystals were obtained,
i.e. N2H6(Sb2F11)2 and N2H6(SbF6)2. No other phases were observed
when different molar ratios of N2H6F2 / SbF5 (1:1, 2:3,1:3) in aHF
were used as starting materials.
Acta Crystallogr., Sect. C 1988, 44, 1329–1331.
[6] B. Frlec, D. Gantar, L. Golicˇ, I. Leban, J. Fluorine Chem. 1984,
24, 271–279.
ˇ
[7] A. Meden, J. Siftar, L. Golicˇ, Acta Crystallogr., Sect. C 1996, 52,
493–496.
[8] P. Benkicˇ, A. Rahten, A. Jesih, L. Pejov, J. Chem. Crystallogr.
2002, 32, 227–235.
[9] P. Klampfer, P. Benkicˇ, M. Ponikvar, A. Rahten, A. Lesar, A.
Jesih, Monatsh. Chem. 2003, 134, 1–9.
[10] H. Barbes, G. Mascherpa, R. Foucade, B. Ducourant, J. Solid
State Chem. 1985, 60, 95–100.
[11] L. Golicˇ, V. Kaucˇicˇ, Acta Crystallogr., Sect. B 1980, 36, 659–661.
ˇ
[12] B. Kojic´-Prodic´, B. Matkovic´, S. Sc´avnicˇar, Acta Crystallogr.,
Sect. B 1971, 27, 635–637.
ˇ
[13] B. Kojic´-Prodic´, S. Sc´avnicˇar, B. Matkovic´, Acta Crystallogr.,
Sect. B 1971, 27, 638–644.
[14] A. Rahten, I. Leban, S. Milic´ev, B. Zemva, J. Crystallogr. Spect.
ˇ
Res. 1990, 20, 9–15.
[15] T. S. Cameron, O. Knop, L. A. MacDonald, Can. J. Chem. 1983,
61, 184–188.
[16] B. Frlec, D. Gantar, L. Golicˇ, I. Leban, Acta Crystallogr., Sect. B
1981, 37, 666–668.
[17] C. Garcia, D. Barbusse, R. Fourcade, B. Ducourant, J. Fluorine
Chem. 1991, 51, 245–256.
[18] P. Benkicˇ, H. D. B. Jenkins, M. Ponikvar, Z. Mazej, Eur. J. Inorg.
Chem. 2006, 2006, 1084–1092.
Crystallization products were immersed in perfluorinated oil (ABCR,
FO5960, melting point 263 K) in a dry-box. Single crystals were se-
lected from the crystallization products under the microscope outside
the dry-box and transferred into the cold nitrogen stream of the dif-
fractometer.
[19] T. Steiner, Angew. Chem. Int. Ed. 2002, 41, 48–76.
[20] Z. Mazej, J. Fluorine Chem. 2004, 125, 1723–1733.
[21] A. I. Popov, M. D. Valkovskii, V. F. Suhoverhov, Zh. Neorg.
Khim. 1990, 35, 2831–2836.
4.4. Crystal Structure Determination of N2H6(Sb2F11)2 and
N2H6(SbF6)2
Single-crystal data for both compounds were collected on a Gemini A
diffractometer equipped with an Atlas CCD detector, using graphite
monochromatized Mo-Kα radiation. Data were treated using the Crys-
[22] S. Seidel, K. Seppelt, Science 2000, 290, 117–118.
[23] W. A. S. Nandana, J. Passmore, P. S. White, C.-M. Wong, Inorg.
Chem. 1990, 29, 3529–3538.
alis software suite program package.[30] Structures were solved by [24] H. Willner, F. Aubke, Organometallics 2003, 22, 3612–3633.
charge flipping method using Superflip[31] program (Olex crystallo-
graphic software[32]) and refined with SHELXL-2013[33] software, im-
plemented in program package WinGX.[34] Hydrogen atoms were lo-
calized from peaks of electron density in different Fourier maps. Be-
cause of varied N–H distances the final refinement was performed with
geometrical restrictions for hydrogen atoms positions. The figures
were prepared using DIAMOND 3.1 software.[35]
[25] I. H. T. Sham, B. O. Patrick, B. von Ahsen, S. von Ahsen, H.
Willner, R. C. Thompson, F. Aubke, Solid State Sci. 2002, 4,
1457–1463.
ˇ
[26] Z. Mazej, P. Benkicˇ, K. Lutar, B. Zemva, J. Fluorine Chem. 2001,
112, 173–183.
[27] PTFE valves were constructed and made at Jozˇef Stefan Institute
in a similar way as shown in: O’Donnelll, The Chemistry of
Fluorine; in Comprehensive Inorganic Chemistry, Pergamon
Press, Oxford, 1973, p. 1918.
ˇ
Further details of the crystal structure investigations may be obtained
[28] Z. Mazej, B. Zemva, J. Fluorine Chem. 2005, 126, 1432–1434.
from the Fachinformationszentrum Karlsruhe, 76344 Eggenstein- [29] W. M. McBride, R. A. Henry, S. Skolnik, Anal. Chem. 1951, 23,
890–893.
Leopoldshafen, Germany (Fax: +49-7247-808-666; E-Mail:
crysdata@fiz-karlsruhe.de, http://www.fiz-karlsruhe.de/request for de-
posited data.html) on quoting the depository numbers CSD-429156
(N2H6(Sb2F11)2) and -429157 (N2H6(SbF6)2).
[30] CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release
14–01–2014 CrysAlis171.NET), 2014.
[31] L. Palatinus, G. Chapuis, J. Appl. Crystallogr. 2007, 40, 786–790.
[32] O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard, H.
Puschmann, J. Appl. Crystallogr. 2009, 42, 339–341.
[33] G. M. Sheldrick, Acta Crystallogr., Sect. C 2015, 71, 3–8.
[34] L. J. Farrugia, J. Appl. Crystallogr. 2012, 45, 849–854.
[35] DIAMOND v3.1, Crystal Impact GbR, Bonn, Germany, 2005.
Acknowledgements
The authors gratefully acknowledge the financial support from the
Slovenian Research Agency (ARRS) within the research program:
P1–0045 Inorganic Chemistry and Technology.
Received: February 25, 2015
Published Online: April 14, 2015
Z. Anorg. Allg. Chem. 2015, 1216–1219
1219
© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim