A spatially separated [KBr6]5- anion in the cyanido-bridged uranium(IV) compound [U2(CN)3(NH3)14]5+[KBr6]5-·NH3

Article abstract of DOI:10.1515/znb-2019-0161

The reaction of uranium tetrabromide with potassium cyanide in anhydrous liquid ammonia at room temperature leads to the formation of brown crystals of [U₂(CN)₃(NH₃)₁₄]⁵⁺ [KBr₆]^5- · NH₃. We determined the crystal structure of the compound by single crystal X-ray diffraction. To the best of our knowledge it contains the unprecedented spatially separated [KBr₆]^5- anion and presents the first uranium(IV) cyanide compound which forms a layer structure. The compound crystallizes in the trigonal space group P3 m1 (No. 164) with a = 10.3246(13), c = 8.4255(17) ?, V = 777.8(3) ?³, Z = 1 at T = 100 K and is well described with the Niggli formula ² _∞[U(CN)_3/2(NH₃)_7/1]₂[KBr_6/1].

Full text of DOI:10.1515/znb-2019-0161

Z. Naturforsch. 2019; aop
HA. Lsarps DaeutbinaelrlayndsFloeripanaKrraaust*ed [KBr6]5− anion in the
cyanido-bridged uranium(IV) compound
[U2(CN)3(NH3)14]5+[KBr6]5−ꢀ·ꢀNH3
https://doi.org/10.1515/znb-2019-0161
tetracyanidoplatinate(II) complexes like {U2(H2O)10(O)
[Pt(CN)4]3}ꢀ·ꢀ4H2O, also some CN−-containing compounds
with organic ligands are described [15, 16]. These are, for
example [UN*3CN] (N*ꢀ=ꢀN(SiMe3)2) or [M][(UN*3)2(μ-CN)]
(Mꢀ=ꢀK(18-crown-6), N*ꢀ=ꢀN(SiMe3)2), of which the crystal
structures have been determined [8, 9]. Also, some CN−-
bridged uranium complexes with sterically demand-
ing ligands are known [6, 7, 9, 17–19]. To the best of our
knowledge a pseudo-binary uranium cyanide, such as
U(CN)4, is still unknown. Our attempts and investiga-
tions on the synthesis of uranium cyanides in liquid
ammonia led to the discovery of the light-green com-
pound [UCl3(CN)ꢀ·ꢀ4NH3], obtained from UCl4 and NaCN in
liquid NH3 [3, 20]. The reaction of UCl4 with one equivalent
of KCN in liquid ammonia at room temperature gave green
crystals of [U(CN)(NH3)8]Cl3ꢀ·ꢀNH3 [20]. Uranium tetraio-
dide, UI4, reacts with one equivalent of KCN leading to a
compound with infinite chains of cyanido- and amido-
bridged uranium atoms in the crystal structure [20].
Hexaamminetricyanidouranium(IV) iodide [U(CN)3(NH3)6]I
can be obtained by increasing the concentration of KCN
and heating the reaction mixture [20]. Here we present
the synthesis and crystal structure of the cyanido bridged
uranium(IV) compound [U2(CN)3(NH3)14]5+[KBr6]5−ꢀ·ꢀNH3 that
contains, to the best of our knowledge, an unprecedented
spatially separated [KBr6]5− anion.
Received October 14, 2019; accepted October 23, 2019
Abstract: The reaction of uranium tetrabromide with
potassium cyanide in anhydrous liquid ammonia at room
temperature leads to the formation of brown crystals of
[U2(CN)3(NH3)14]5+ [KBr6]5−ꢀ·ꢀNH3. We determined the crystal
structure of the compound by single crystal X-ray diffrac-
tion. To the best of our knowledge it contains the unprece-
dented spatially separated [KBr6]5− anion and presents the
first uranium(IV) cyanide compound which forms a layer
structure. The compound crystallizes in the trigonal space
̅
group P3m1 (No. 164) with aꢀ=ꢀ10.3246(13), cꢀ=ꢀ8.4255(17) Å,
Vꢀ=ꢀ777.8(3) Å3, Zꢀ=ꢀ1 at Tꢀ=ꢀ100 K and is well described with
2 
∞ 
 


the Niggli formula U(CN)3 (NH3 )
KBr .

71  
61 
2
2 
Keywords: ammonia; bromide; crystal structure; cyanide;
uranium.
Dedicated to: Professor Dr. rer. nat. Dr. h.c. mult. Arndt Simon on
the occasion of his 80th birthday.
1 Introduction
While a multitude of cyanide complexes of the transition
metals are known [1, 2], only a few cyanido complexes of
uranium(IV) have been reported [3–10]. The first actinoid
compound containing cyanide anions was K2[UO2(CN)4]
described by Aloy, followed by K2[UO2(CN)2(NO3)2] [11,
12]. However, the existence of both compounds was
doubted and literature suggests to regard them as non-
existent [13, 14]. Besides uranium compounds contain-
ing hexacyanido complexes of group eight elements,
such as {[U(H2O)10][M(CN)6]} (MIIꢀ=ꢀFe, Ru, Os), and some
2 Results and discussion
The reaction of UBr4 with KCN dissolved in liquid ammonia
was carried out in a sealed “bomb tube” at room tempera-
ture. Over 6 months of storage and crystallization time
some dark brown crystals grew of which the com-
position was evidenced by X-ray diffraction as
tetradecaamminetricyanido-κC,κN-diuranium(IV)
hexabromidopotassiate(I) ammonia(1/1) [U2(CN)3(NH3)14]5+
[KBr6]5−ꢀ·ꢀNH3. The formation of this compound can be
described by eq. (1).
*Corresponding author: Florian Kraus, Fachbereich Chemie,
Philipps-Universität Marburg, Hans-Meerwein-Str. 4, 35032
Marburg, Germany, E-mail: f.kraus@uni-marburg.de, florian.kraus@
chemie.uni-marburg.de
H. Lars Deubner: Fachbereich Chemie, Philipps-Universität Marburg,
Hans-Meerwein-Str. 4, 35032 Marburg, Germany
NH3(I)
2 UBr4 +15 NH3 + 3 KCN →[U2 (CN)3(NH)14 ]5+
[KBr ]5− · NH3 + 2 KBr
(1)
6
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2ꢁ
ꢁH. L. Deubner and F. Kraus: A spatially separated [KBr6]5−ꢁ anion
ꢀꢀꢀꢁ
The compound crystallizes in the trigonal space group of this compound contains the [KBr6]5− anion and the
P3m1 (No. 164) with aꢀ=ꢀ10.3246(13), cꢀ=ꢀ8.4255(17) Å, [U2(CN)3(NH3)14]5+ cation, as well as an ammonia molecule
̅
Vꢀ=ꢀ777.8(3) Å3 and Zꢀ=ꢀ1 at Tꢀ=ꢀ100 K. Selected crystal- of crystallization. The [KBr6]5− anion and the coordination
lographic data and details of the structure determina- sphere of the U(IV) cation are shown in Fig. 1.
tion are available from Table 1. Table 2 contains Wyckoff
The spatially separated [KBr6]5− anion is, to the best
positions and atom coordinates. The crystal structure of our knowledge, not described in the literature to
date. However, a inversely comparable species has been
observed in the compound [K17(Sb8)2(NH2)]ꢀ·ꢀ17.5NH3,
where [(H2N)K6] octahedra are present that however
Table 1:ꢀSelected crystallographic data and details of the structure
form straight, infinite chains through trans-corner con-
nections. Thus, a similarity to the crystal structure of
KNH2 was noted [21]. In our case, the [KBr6]5− anion is
spatially separated and contains a potassium atom (1a,
determination of [U2(CN)3(NH3)14]5+[KBr6]5−ꢁ·ꢁNH3.
Formula
[U2(CN)3(NH3)14][KBr6]ꢁ·ꢁNH3
Molar mass/gꢁ·ꢁmol−1
Space group (No.)
a/Å
1328.09
̅
P3m1 (164)
̅
3m.) as the central atom, which is surrounded by six
10.3246(13)
8.4255(17)
777.8(3)
1
symmetry-equivalent bromide anions (6i, .m.) in the
shape of a distorted octahedron. The K–Br distances of
such a moiety are therefore all equal with 3.2684(19) Å.
This distance is in good agreement with K–Br distances
observed for pure KBr (3.289(6) Å, Tꢀ=ꢀ293 K) [22]. Intera-
tomic distances are available from Table 3. In the com-
pound K2ZnBr4, where the coordination polyhedron
c/Å
V/Å3
Z
Pearson symbol
ρcalcd./gꢁ·ꢁcm−3
μ/mm−1
hP108
2.84
18.3
Color
Brown
Crystal habitus
Crystal size/mm3
T/K
Block
+
around K is a trigonal prism, the K−Br distances agree
0.1ꢁꢁ·ꢁꢁ0.1ꢁꢁ·ꢁꢁ0.05
100(2)
with 3.240–3.420 Å (Tꢀ=ꢀ125 K) [23, 24]. An octahedral
coordination polyhedron for potassium cations and
bromide anions is also present in the compound KInBr3
[25]. There, the K–Br distances of 3.182(9) and 3.284(9) Å
are also comparable with those in the spatially separated
anion presented here. The Br–K–Br angles in the dis-
torted coordination octahedron of the [KBr6]5− anion are
102.52(4) and 77.48(4)°; in good agreement with reported
data (KInBr3: 105.09 and 74.01°) [25]. Overall, the shape
of the spatially separated [KBr6]5− anion corresponds
well to the literature.
Radiation; λ/Å
No. of reflections
θ range/°
Range of Miller indices hkl
Absorption correction
MoKα; 0.71073
14745
3.322–29.357
14, 14, 11
multi-scan
0.430; 0.204
0.995
816
0.0556; 0.0572
39
T
max; Tmin
Completeness of the data set
No. of unique reflections
R
int; Rσ
No. of parameters
No. of restrains
No. of constrains
S (all data)
0
0
The uranium atom occupies the Wyckoff position
2d (3m.) and is surrounded by seven ammine ligands
and three cyanido ligands. The coordination polyhe-
dron can be described as a slightly distorted spheno-
corona (Johnson solid J86). This sphenocorona, with a
1.247
R(F) (Iꢁ>ꢁ2 σ(I); all data)
wR(F2) (Iꢁ>ꢁ2σ(I); all data)
Extinction coefficient
Δρmax; Δρmin/eꢁ·ꢁÅ−3
0.0555; 0.0571
0.1360; 0.1413
0.0102(18)
2.57; −2.53
Table 2:ꢀAtomic coordinates and equivalent isotropic displacement parameters Uiso for [U2(CN)3(NH3)14]5+[KBr6]5−ꢁ·ꢁNH3.
Atom
Wyckoff position
x
y
z
U
iso/Å2
S.O.F.
U(1)
N(1)
C(1)
N(2)
N(3)
N(4)
N(5)
K(1)
Br(1)
2d
6i
1/3
0.4707(7)
0.4707(7)
1/3
2/3
–x
–x
2/3
–x
2x
0
0.35808(10)
0.4790(14)
0.4790(14)
0.651(2)
0.1310(14)
0.3585(16)
1/2
0.0188(4)
0.021(2)
1
0.5
0.5
1
6i
0.021(2)
2d
6i
6i
1b
1a
6i
0.020(4)
0.4320(7)
0.1870(7)
0
0.025(2)
1
0.028(3)
1
0.061(13)
0.0341(18)
0.0417(5)
1
0
0
0
1
0.16461(11)
–x
0.8313(2)
1
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H. L. Deubner and F. Kraus: A spatially separated [KBr6]5−ꢁ anionꢂ
ꢁꢀꢀꢀ
ꢂ3
Fig. 1:ꢀSection of the crystal structure of [U2(CN)3(NH3)14]5+[KBr6]5−ꢁ·ꢁNH3, showing the octahedron-like [KBr6]5− anion (left) and the coordination
of the U(IV) cation (right). The displacement ellipsoids are shown at the 70% probability level at Tꢁ=ꢁ100 K. As some of the H atoms show site
disorder, only one set of positions is shown.
Table 3:ꢀSelected interatomic distances d and their multiplicities m
for [U2(CN)3(NH3)14]5+[KBr6]5−ꢁ·ꢁNH3.
Atom1
U(1)
Atom2
m
d/Å
N/C(1)
N(2)
N(3)
N(4)
N/C(1)
Br(1)
3
1
3
3
1
6
2.659(13)
2.47(2)
2.603(12)
2.616(13)
1.11(3)
N/C(1)
K(1)
3.2684(19)
mild distortion of its top quadrangle is shown in Fig. 2.
The three disordered cyanido ligands are κC,κN-bridging
two symmetry-equivalent uranium atoms. The C≡N bond
length of the disordered cyanido ligand is 1.11(3) Å and
despite the disorder it agrees well with C≡N bond lengths
of cyanido ligands described in the literature [26–29].
Because of space group symmetry, the C and N atoms
of the cyanide anion are indistinguishable and a statis-
tical distribution with a 50:50 mixed site occupancy of
the atom position 6i (.m.) was applied in the refinement.
Fig. 2:ꢀSection of the crystal structure of
[U2(CN)3(NH3)14]5+[KBr6]5−ꢁ·ꢁNH3, showing the coordination sphere
of the uranium atom, which is surrounded by ten ligands in the
shape of a slightly distorted sphenocorona (Johnson solid J86). A
view along the trigonal prism of the sphenocorona is selected. The
The cyanide anion resides symmetrically in between the displacement ellipsoids are shown at the 70% probability level at
Tꢁ=ꢁ100 K.
bridged U atoms. The U–N distances for the seven ammine
ligands range from 2.47(2) to 2.659(13) Å and are also in
good agreement with distances observed for ammine
ligands in the uranium-ammonia system [20]. Because layer is shown in Fig. 3 left. As every sphenocorona is con-
of the different distances between the uranium atom and nected to three others, a motif of packed sphenocoronas
the ten ligands, the sphenocorona is slightly distorted. is obtained that reminds of the arrangement of As atoms
As the U atoms are bridged by the cyanido ligands, the in the crystal structure of grey arsenic (Fig. 3 right), which
complex cation forms corrugated infinite layers paral- is best seen when viewed parallel to the c axis. Overall,
lel to the ab plane. This connection can be described by the sphenocoronas show AB stacking, that is, the AB
layers are stacked directly above each other and channels
2 





the Niggli formula
U(CN)3 (NH3 )7 . A section of one

parallel to the c axis result (Fig. 3 right).

1 
2

∞ 

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4ꢁ
ꢁH. L. Deubner and F. Kraus: A spatially separated [KBr6]5−ꢁ anion
ꢀꢀꢀꢁ
2




Fig. 3:ꢀSection of the crystal structure showing a corrugated
U(CN)3 (NH3 )7 layer (left) and a view along the c axis (right).
{
}

1 
2
∞
The [KBr6]5− anions fill the octahedral voids, with the
potassium atom K(1) occupying the Wyckoff position 1a
̅
(3m.). The complex anion can be described by the Niggli
0 








KBr6
.
The motif of the arrangement of
formula

1 
∞ 
sphenocoronas and [KBr6]5− anions corresponds overall
to an ABC-type stacking. Leaving the Br, C, and N atoms
aside and looking only on the arrangement of the K and
U atoms, one recognizes that the K atoms are surrounded
octahedron-like by U atoms. These octahedra reside in
the ab planes and share common edges correspond-
Fig. 4:ꢀSection of the crystal structure of
[U2(CN)3(NH3)14]5+[KBr6]5−ꢁ·ꢁNH3. The [KBr6]5− anions are shown as dark
green polyhedra. Displacement ellipsoids are shown at the 70%
probability level at Tꢁ=ꢁ100 K, H atoms isotropic with arbitrary radii.
2 







KU6
.
The arrangement of
ing to the Niggli formula


3 
∞ 
the potassium and uranium atoms reminds of the Ag2F H atoms of the ammonia molecules of crystallization could not be
structure type [30]. The ammonia molecules of crystalli-
zation, with the N(5) atom on the 1b (3m.) position, are
located.
̅
thus also surrounded octahedron-like by six uranium
atoms, however these octahedra are strongly compressed
along the threefold symmetry axis parallel to the crystal-
range from 3.377(10) to 3.642(8) Å. This is in good agree-
ment with known N–Hꢀ·ꢀ·ꢀ·ꢀBr hydrogen bonds for example
in [Co(NH3)6]Br(S2O3)ꢀ·ꢀH2O (3.509(4) to 3.539(3) Å, Tꢀ=ꢀ295 K)
or in [CoCO3(NH3)5]Brꢀ·ꢀH2O (3.41–3.63 Å) [31, 32].
2 







lographic c axis. These polyhedra form
NU6 layers


3 
∞ 
which reside at zꢀ=ꢀ1/2 parallel to the ab plane. Thus, the
2 








NU6
layers of
octahedra are sharing common faces

3 
∞ 
3 Conclusions
2 



KU6
with the
octahedra. The crystal structure of the



3 
Single crystals of [U2(CN)3(NH3)14]5+[KBr6]5−ꢀ·ꢀNH3 (P3m1,


̅
∞ 

compound is shown in Fig. 4.
No. 164) were obtained by the reaction of UBr4 and KCN
Between the layers of the interconnected uranium dissolved in liquid ammonia at room temperature over
atoms and the spatially separated [KBr6]5− anions the only several months of crystallization time. The crystal struc-
attractive interactions are N–Hꢀ·ꢀ·ꢀ·ꢀBr hydrogen bonds. The ture of this compound has been determined and found to
hydrogen atoms of the ammine ligands (N(2), N(3) and contain two peculiar building units: (i) The uranium atoms
N(4)) form hydrogen bonds to the bromine atoms Br(1). are coordinated by ten ligands in total of which seven are
The donorꢀ·ꢀ·ꢀ·ꢀacceptor distances of these hydrogen bonds ammine and three are cyanido ligands. The coordination
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H. L. Deubner and F. Kraus: A spatially separated [KBr6]5−ꢁ anionꢂ
ꢁꢀꢀꢀ
ꢂ5
sphere of the U atom is described best as a sphenocorona.
The connection of the κC,κN-cyanido bridged uranium
4.4 Single-crystal X-ray diffraction
atoms leads to the formation of infinite corrugated layers A crystal of the title compound was selected under nitro-
of sphenocoronas. (ii) The unprecedented spatially sepa- gen-cooled, pre-dried perfluorinated oil and mounted
rated, octahedron-like [KBr6]5− anion could be observed using a MiTeGen loop. Intensity data of a suitable crystal
for the first time.
was recorded with an IPDS 2T diffractometer (STOE & Cie).
The diffractometer was operated with MoKα radiation
(λꢀ=ꢀ0.71073 Å, graphite monochromator) and equipped
with an image plate detector. Evaluation, integration and
reduction of the diffraction data was carried out using the
X-Area software suite [34]. A numerical absorption correc-
tion was applied with the modules X-Shape and X-Red32
of the X-Area software suite. The structure was solved with
dual-space methods (Shelxt-2014/5) and refined against
F2 (Shelxl-2014/7) [35, 36]. All atoms were refined with
anisotropic displacement parameters. The highest resid-
ual electron density after the final refinement was 1.142 Å
distant from atom K(1).
4 Experimental section
All work was carried out excluding moisture and air in
an atmosphere of dried and purified argon (5.0, Praxair)
using high vacuum glass lines and a glovebox (MBraun).
The glass vessels were flame dried several times under
vacuum before being used. Aluminum bromide (Alfa
Aesar, 98%) was purified by sublimation in vacuo. Alu-
minum (Fluka, purum >99%), as well as uranyl nitrate
(Riedel de Haën, zur Analyse), was used as supplied.
CCDC 1959129 contains the supplementary crystallo-
graphic 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.
4.1 Synthesis of UO2
12.8 g of UO2(NO3)2ꢀ·ꢀ6H2O (25.4 mmol) was decomposed
to 7.13 g U3O8 (8.47 mmol) by heating to 700°C in air for
12 h inside an open silica test tube. The black product was
powdered in air and reduced in a stream of hydrogen at
800°C for 8 h to obtain 6.86 g (24.9 mmol, 98%) of phase
pure UO2.
Acknowledgement: We thank the Deutsche Forschungsge-
meinschaft for funding and Dr. Matthias Conrad, Marburg,
for helpful discussions.
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4.2 Synthesis of UBr4
UBr4 was synthesized according to the literature [33]. An
ampoule was charged with 1088 mg UO2 (4 mmol) and
2150ꢀ+ꢀ65 mg AlBr3 (8 mmolꢀ+ꢀtransport agent) and flame
sealed under vacuum (1ꢀ×ꢀ10−3 mbar). The starting materi-
als were reacted at 250°C for 12 h before the transport reac-
tion was conducted with a source temperature of 350°C
and a sink temperature of 230°C. One thousand nine
hundred and seventy-eight milligram (4.3 mmol, 86%) of
large brown plate-shaped crystals of UBr4 were obtained
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4.3 Synthesis of [U2(CN)3(NH3)14]5+[KBr6]5−ꢀ·ꢀNH3
Thirty milligram of UBr4 (0.05 mmol) and 13 mg of KCN
(0.2 mmol, 4 eq.) were reacted with liquid ammonia in a
flame sealed glass ampoule (bomb tube made of borosili-
cate glass, 6 mm diameter with 1.5 mm wall thickness) at
room temperature for 6 months.
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6ꢁ
ꢁH. L. Deubner and F. Kraus: A spatially separated [KBr6]5−ꢁ anion
ꢀꢀꢀꢁ
[14] J. I. Bullock, J. Inorg. Nucl. Chem. 1967, 29, 2257–2264.
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Z. Naturforsch.ꢂ
ꢂ2019 | Volume x | Issue x(b)
Graphical synopsis
H. Lars Deubner and Florian Kraus
A spatially separated [KBr6]5− anion in the
cyanido-bridged uranium(IV) compound
[U2(CN)3(NH3)14]5+[KBr6]5−ꢀ·ꢀNH3
https://doi.org/10.1515/znb-2019-0161
Z. Naturforsch. 2019; x(x)b: xxx–xxx
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