K4Ti3Te9 - A new pseudo one-dimensional polyanionic alkali chalcogenometallate(IV)

Article abstract of DOI:10.1515/znb-2003-0705

Lustrous black needle shaped single crystals of K₄Ti ₃Te₉ were obtained by reacting K₂Te with the corresponding elemental components at 1000°C. K₄Ti ₃Te₉ is monoclinic, mP64, s.g. P2₁/c (No. 14), Z = 4 with a = 9.052(2), b = 8.088(1), c = 29.465(9) A?, β = 92.35(1)°. The crystal structure was determined from diffractometer data and refined to a conventional R value of 0.035 (2840 F_o's, 146 variables). The compound contains undulating polyanionic chains built up by severely distorted TiTe₆ octahedra sharing opposite faces which run parallel to [100] and are arranged in a hexagonal rod packing. The translation period comprises three octahedra. The most striking feature of this compound is the formation of two ditelluride groups per formula unit with unusually long Te-Te distances of 2.960(2) and 3.025(2) A?, respectively. All other Te-Te distances start at 3.2 A?. The nearest homonuclear neighbours of the two pairs are at 3.215(2) and 3.333(2) A? apart. Ti-Te bond lengths range from 2.700(3) to 2.841(3) A? with an average value of 2.772(4) A? for all three crystallographically independent titanium atoms. The alkali cations are irregularly coordinated by 7 to 9 tellurium atoms.

Full text of DOI:10.1515/znb-2003-0705

K4Ti3Te9 – A New Pseudo One-Dimensional Polyanionic
Alkali Chalcogenometallate(IV)
Andreas Kolb and Kurt O. Klepp
Department of General and Inorganic Chemistry, University of Linz,
Altenbergerstr. 69, A-4040 Linz, Austria
Reprint requests to Prof. Kurt O. Klepp. E-mail: kurt.klepp@jku.at
Z. Naturforsch. 58b, 633 – 638 (2003); received March 14, 2003
Lustrous black needle shaped single crystals of K4Ti3Te9 were obtained by reacting K2Te with
the corresponding elemental components at 1000 ◦C. K4Ti3Te9 is monoclinic, mP64, s. g. P21/c
◦
˚
(No. 14), Z = 4 with a = 9.052(2), b = 8.088(1), c = 29.465(9) A, β = 92.35(1) . The crystal struc-
ture was determined from diffractometer data and refined to a conventional R value of 0.035 (2840
Fo’s, 146 variables). The compound contains undulating polyanionic chains built up by severely
distorted TiTe6 octahedra sharing opposite faces which run parallel to [100] and are arranged in a
hexagonal rod packing. The translation period comprises three octahedra. The most striking feature
of this compound is the formation of two ditelluride groups per formula unit with unusually long
˚
˚
Te-Te distances of 2.960(2) and 3.025(2) A, respectively. All other Te-Te distances start at 3.2 A.
˚
The nearest homonuclear neighbours of the two pairs are at 3.215(2) and 3.333(2) A apart. Ti-Te
˚
˚
bond lengths range from 2.700(3) to 2.841(3) A with an average value of 2.772(4) A for all three
crystallographically independent titanium atoms. The alkali cations are irregularly coordinated by 7
to 9 tellurium atoms.
Key words: Chalcogenides, Polyanionic Chains, Group IVa Metal Compounds
Introduction
resents the lowest member of this polyanionic series
so far.
A large number of polychalcogenides AmTInVQo
(A = Na – Cs, Tl; T = Ti, Zr, Hf; Q = S, Se, Te)
with pseudo one-dimensional structures has been re-
ported during the last decade. They comprise the
sulfides, Tl2TiS4 [1], K2ZrS4, Rb2ZrS4, Rb2HfS4
[2], K2Ti2S9 [3], Cs2Ti2S9 [4], A4Ti3S14, (A = K –
Cs) [5, 6], Cs4Zr3S14 [7], Rb4Hf3S14 [6], the se-
lenides Na2Ti2Se8 [8], Cs4Ti3Se13 [6], Na2Ti2Se9
[9], Rb4Ti3Se13 [10], K4Hf3Se14 [7], Rb4Zr3Se14,
Rb4Hf3Se14 [10], Cs4Zr3Se14 [6], Cs4Hf3Se14 [6],
K4Zr3Se15 [11] and finally the tellurides Rb3Ti3Te11
[12], Cs3Ti3Te11 [13], Cs4Hf3Te13 [14], Cs5Hf5Te26
[15], Cs4Zr3Te16 [16], Rb4Zr3Te16 [17], Rb4Hf3Te16
[10], K4Zr3Te17 [14] and K4Hf3Te17 [18]. Out of these
the tellurides merit particular interest since they show
the widest range of polyanionic compositions and are
invariably characterized by partial Te-Te bonds. It was
therefore of interest to find out whether this pecu-
liarity persists at even lower tellurium contents. This
led to the preparation of K4Ti3Te9 – which coming
close to the normal valence composition K2TiTe3 rep-
Table 1. Crystallographic data for K4Ti3Te9.
Pearson Symbol
mP64
˚
a[A]
9.052(2)
8.008(1)
29.465(9)
92.35(1)
P21/c (No. 14)
4
˚
b[A]
˚
c[A]
β [◦]
Space group
Z
3
˚
V [A ]
dx [gcm−3
2134.1
4.51
]
Mr
1448.51
139.50
µ(Mo-Kα ) [cm−1
]
Structure refinement:
Unique reflections
Observed reflections
Cutoff
4620
2840
3.00σ(F )2
o
Variables
146
R = ||F |−|F ||/ |F |
0.037
∑
∑
o
c
o
ꢀ
ꢁ1/2
o
2
2
Rw
=
w||F |−|F || / w|F |
0.035
∑
∑
o
c
ꢂ
ꢃ−1/2
w = σ(Fo2)2 +(0.05Fo2)2
−3
˚
Residual electron density [eA
]
1.69/−0.67
c
0932–0776 / 03 / 0700–0633 $ 06.00 ꢀ 2003 Verlag der Zeitschrift fu¨r Naturforschung, Tu¨bingen · http://znaturforsch.com
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634
A. Kolb – K. O. Klepp · K4Ti3Te9
Table 2. Positional parameters and thermal displacement factors for K Ti3Te9. (All atoms lie on the Wyckoff position 4e.)
4
∗
Atom
K(1)
K(2)
K(3)
K(4)
x
y
z
U11
U22
U33
U12
U13
U23
Beq
0.3881(5) 0.2360(5) 0.4837(1)
0.9327(5) 0.2093(7) 0.4347(2)
0.1308(5) 0.2352(7) 0.7671(2)
0.5719(5) 0.2174(7) 0.3170(2)
0.036(2)
0.035(2)
0.039(2)
0.040(2)
0.011(1)
0.010(1)
0.009(1)
0.040(3)
0.054(3)
0.066(3)
0.059(3)
0.030(1)
0.034(2)
0.036(2)
0.028(2)
0.041(2)
0.030(2)
0.039(2)
0.026(1)
0.024(1)
0.023(1)
−0.003(2)
0.002(2)
−0.014(2)
−0.003(2)
0.001(1)
−0.001(1)
0.000(1)
0.0012(5)
0.009(2)
−0.002(2)
0.006(2)
−0.010(2)
0.0020(9)
−0.001(1)
0.000(1)
−0.000(2)
−0.007(2)
0.006(2)
0.010(2)
0.002(1)
0.002(1)
−0.000(1)
2.73(8)
3.43(9)
3.6(1)
3.60(9)
1.74(5)
1.71(5)
1.80(5)
Ti(1) 0.9201(3) 0.1853(4) 0.1306(1)
Ti(2) 0.2515(4) 0.2641(4) 0.6271(1)
Ti(3) 0.5831(3) 0.1948(4) 0.1164(1)
Te(1) 0.0670(1) 0.1668(2) 0.05012(4) 0.0178(4) 0.0261(6) 0.0292(5)
0.0047(4) −0.0026(5) 2.30(2)
Te(2) 0.4512(1) 0.1676(2) 0.20012(3) 0.0137(4) 0.0294(6) 0.0257(5) −0.0017(5) −0.0009(4)
Te(3) 0.7386(1) 0.1596(2) 0.69238(4) 0.0142(4) 0.0275(6) 0.0262(5)
Te(4) 0.7709(1) 0.1588(2) 0.55504(4) 0.0160(4) 0.0255(6) 0.0298(5) −0.0000(5)
Te(5) 0.4227(1) 0.0258(1) 0.58892(4) 0.0188(4) 0.0460(8) 0.0186(5) 0.0016(6)
Te(6) 0.0699(1) 0.0272(1) 0.66196(4) 0.0292(5) 0.0417(7) 0.0182(5) −0.0084(6)
0.0066(5) 2.16(2)
0.0018(5) −0.0002(4) −0.0040(5) 2.30(2)
0.0033(4)
0.0024(4)
0.0030(5) 2.15(2)
0.0011(6) 1.88(2)
0.0020(4) −0.0015(6) 1.88(2)
Te(7) 0.6202(1) 0.0108(1) 0.92600(4) 0.0166(4) 0.0394(7) 0.0267(5) −0.0021(5) −0.0006(4) −0.0106(6) 1.79(2)
Te(8) 0.2533(1) 0.0946(1) 0.87759(4) 0.0207(5) 0.0420(7) 0.0251(5)
Te(9) 0.1173(1) 0.9847(1) 0.17529(4) 0.0135(4) 0.0286(5) 0.0302(5) −0.0008(6) −0.0021(3)
0.0004(6) −0.0014(4)
0.0115(6) 1.87(2)
0.0000(6) 1.81(2)
8π2
3
∗Beq
=
U a∗a∗a a .
∑∑
ij
i j
i j
i
j
Table 3. Selected interatomic distances and bond angles for Table 3 (continued).
K4Ti3Te9.
Ti(2)-Te(2)
Ti(2)-Te(6)
Ti(2)-Te(4)
Ti(1)-Ti(3)
2.700(3)
Ti(2)-Te(9)
Ti(2)-Te(7)
Ti(2)-Te(8)
Ti(2)-Ti(3)
2.740(4)
2.788(3)
2.834(3)
3.059(3)
a) Coordination of the alkali cations
2.763(3)
2.801(4)
3.046(5)
K(1)-Te(3)
K(1)-Te(3)
K(1)-Te(1)
K(1)-Te(1)
K(1)-Te(9)
K(1)-Te(8)
K(1)-Te(6)
3.411(5)
3.447(5)
3.486(5)
3.523(5)
3.566(6)
3.635(5)
3.646(5)
K(2)-Te(4)
K(2)-Te(3)
K(2)-Te(6)
K(2)-Te(6)
K(2)-Te(9)
K(2)-Te(1)
K(2)-Te(8)
K(2)-Te(2)
K(2)-Te(8)
3.419(6)
3.603(5)
3.680(6)
3.682(6)
3.751(5)
3.766(5)
3.897(6)
3.924(6)
3.985(6)
Te(6)-Ti(2)-Te(8)
Te(2)-Ti(2)-Te(9)
Te(8)-Ti(2)-Te(9)
Te(2)-Ti(2)-Te(6)
Te(4)-Ti(2)-Te(6)
Te(6)-Ti(2)-Te(9)
Te(6)-Ti(2)-Te(7)
Te(4)-Ti(2)-Te(9)
65.4(1)
85.3(1)
92.2(1)
93.1(1)
94.8(1)
100.1(1)
154.0(2)
164.9(1)
Te(4)-Ti(2)-Te(7)
Te(2)-Ti(2)-Te(4)
Te(7)-Ti(2)-Te(8)
Te(7)-Ti(2)-Te(9)
Te(4)-Ti(2)-Te(8)
Te(2)-Ti(2)-Te(7)
Te(2)-Ti(2)-Te(8)
73.2(1)
91.6(1)
92.4(1)
94.0(1)
96.1(1)
109.9(1)
157.7(1)
K(3)-Te(2)
K(3)-Te(2)
K(3)-Te(4)
K(3)-Te(9)
K(3)-Te(5)
K(3)-Te(4)
K(3)-Te(7)
3.359(5)
3.503(6)
3.532(6)
3.571(6)
3.654(5)
3.656(6)
3.769(6)
K(4)-Te(1)
K(4)-Te(2)
K(4)-Te(5)
K(4)-Te(5)
K(4)-Te(9)
K(4)-Te(4)
K(4)-Te(3)
3.371(6)
3.535(6)
3.586(6)
3.646(6)
3.760(6)
3.805(5)
3.883(6)
Ti(3)-Te(3)
Ti(3)-Te(1)
Ti(3)-Te(5)
2.725(4)
2.763(4)
2.791(3)
Ti(3)-Te(9)
Ti(3)-Te(8)
Ti(3)-Te(7)
2.747(4)
2.780(3)
2.841(3)
Te(5)-Ti(3)-Te(7)
Te(3)-Ti(3)-Te(9)
Te(7)-Ti(3)-Te(8)
Te(3)-Ti(3)-Te(5)
Te(1)-Ti(3)-Te(5)
Te(1)-Ti(3)-Te(7)
Te(5)-Ti(3)-Te(8)
Te(1)-Ti(3)-Te(9)
63.4(1)
82.7(1)
92.4(1)
92.9(1)
94.7(1)
97.7(1)
154.0(2)
166.9(1)
Te(1)-Ti(3)-Te(8)
Te(1)-Ti(3)-Te(3)
Te(7)-Ti(3)-Te(9)
Te(8)-Ti(3)-Te(9)
Te(5)-Ti(3)-Te(9)
Te(3)-Ti(3)-Te(8)
Te(3)-Ti(3)-Te(7)
78.4(1)
91.1(1)
92.6(1)
93.2(1)
97.1(1)
112.1(1)
155.2(1)
b) Geometry of the 1∞[Ti3Te9]4−-chain
Ti(1)-Te(1)
Ti(1)-Te(2)
Ti(1)-Te(6)
Ti(1)-Ti(2)
2.723(4)
2.768(4)
2.797(5)
3.022(5)
Ti(1)-Te(4)
Ti(1)-Te(3)
Ti(1)-Te(5)
Ti(1)-Ti(3)
2.737(4)
2.788(4)
2.811(5)
3.046(5)
˚
c) Te-Te distances up to 3.8 A
Te(3)-Ti(1)-Te(6)
Te(2)-Ti(1)-Te(3)
Te(2)-Ti(1)-Te(6)
Te(2)-Ti(1)-Te(4)
Te(1)-Ti(1)-Te(5)
Te(1)-Ti(1)-Te(6)
Te(5)-Ti(1)-Te(6)
Te(1)-Ti(1)-Te(2)
70.3(1)
88.6(1)
90.9(1)
91.5(2)
95.2(1)
98.0(2)
157.3(1)
170.3(2)
Te(2)-Ti(1)-Te(5)
Te(1)-Ti(1)-Te(3)
Te(3)-Ti(1)-Te(5)
Te(1)-Ti(1)-Te(4)
Te(4)-Ti(1)-Te(6)
Te(4)-Ti(1)-Te(5)
Te(3)-Ti(1)-Te(4)
75.2(1)
90.6(2)
91.2(1)
91.6(1)
95.5(1)
102.6(2)
165.8(2)
Te(5)-Te(7)
Te(3)-Te(6)
Te(2)-Te(5)
Te(3)-Te(9)
2.960(2)
3.215(2)
3.403(2)
3.616(1)
Te(6)-Te(8)
Te(4)-Te(7)
Te(1)-Te(8)
Te(2)-Te(9)
3.025(2)
3.333(2)
3.503(2)
3.687(1)
icals). As a first step of the synthesis, K2Te was obtained
by reacting the constituent elements in liquid ammonia. Sto-
ichiometric amounts of the powdered educts were intimately
mixed in an argon glove box and sealed into a silica am-
poule under a vacuum of 10−2 Pa. T◦hermal treatment con-
sisted of gradually heating to 1000 C, annealing for 1 d
Experimental Section
The title compound was prepared from high purity ele-
ments (K: 99.9%, Ti: 99.6% and Te 99.999%; Strem Chem-
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A. Kolb – K. O. Klepp · K4Ti3Te9
635
Fig. 1. Projection of the crystal structure of
K4Ti3Te9 showing the hexagonal rod packing
of the anionic chains. The K atoms are rep-
resented by full, Ti and Te atoms by small or
large shaded circles, respectively.
Fig. 2. Bond lengths in the [Ti3Te9]4−
˚
chain up to 3.2 A. Homonuclear bonds are
represented by full rods.
followed by◦controlled cooling to ambient temperature at a sity data were corrected for Lorentz- and polarization effects.
rate of −2 C h−1. The reaction product consisted of lus- Merging symmetry equivalent reflections (Rint = 0.042) led
trous needle shaped crystals which were very sensitive to to a unique set of 4620 observations out of which 2840 with
air and humidity and had hence to be handled under inert I > 3σ(I) were considered as significant.
conditions.
The crystal structure was solved by direct methods (Mul-
For the structure determination a specimen with the di- tan 88 [19]) yielding the positions of the heavier atoms. The
mensions 0.2 × 0.06 × 0.025 mm3 was selected, embedded potassium atoms were located from subsequent difference
in a thin walled glass capillary and transferred to a kappa Fourier syntheses. Anisotropic refinement of the complete
diffractometer (Nonius Turbo CAD4) operated with graphite structure converged rapidly to a final residual of 0.037. A
˚
monochromated Mo-Kα -radiation (λ = 0.71073 A).
final difference Fourier map was featureless. All calculations
Results of preliminary crystallographic investigations in- were performed with programs of the MolEN-crystallogra-
dicated monoclinic symmetry; systematic extinctions: 0k0 : phic software package [20]. Absorptions effects were taken
k = 2n, h0ꢀ: ꢀ = 2n unambiguously led to space group P21/c. into account by empirical correction [21].
The collection of◦the intensity data was performed at room
Precise lattice constants were obtained by refining the set-
temperature (21(1) C) over one quadrant of the reflection ting angles of 25 reflections with 28◦ ≤ 2ϑ ≤ 36◦. They
sphere (0 < 2ϑ < 54◦, ω − 2ϑ scans, maximum scan time are given in Table 1 together with other crystallographic
80 s, scan width 1.20◦ + 0.35◦ tanϑ). Crystal and orienta- data. Positional and thermal displacement parameters are
tional stability were monitored through the periodic determi- given in Table 2. Further details on the structure determi-
nation of three control reflections which, however, showed nation can be obtained from the Fachinformationszentrum
only statistical fluctuations of their intensities. The inten- Karlsruhe, D-76344 Eggenstein- Leopoldshafen (FAX +49
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636
A. Kolb – K. O. Klepp · K4Ti3Te9
Fig. 3. Detailed views
of the chalcogen coor-
dination of the cations
K1 – K4.
(0)7247-808-666; e-mail: crysdata@fiz-karlsruhe.de) under clear interactions. The individual Ti—Te distances lie
˚
CSD 391207.
in the range of 2.700(3) to 2.841(3) A, the average Ti—
˚
Te bond distance is 2.772(4) A and is identical for all
Ti-atoms within experimental errors. A slightly higher
value (dTi−Te = 2.789(2) A) is found in the anionic
Results and Discussion
˚
chains of Tl2TiTe3 [22]. As can be seen from Fig. 2
the main reason for the distortion of the Ti—Te octa-
hedra is the formation of two ditelluride pairs (Te(5)–
Te(7)) and (Te(6)–Te(8))which act as bidentate ligands
on Ti(3) and Ti(2), respectively. Surprisingly the Te–
K4Ti3Te9 crystallizes with a new structure type
which is characterized by the formation of infinite an-
ionic chains, 1 [Ti3Te9]4−. These chains traverse the
∞
structure in the a-direction and are packed in the sense
of a hexagonal rod packing which yields triangular
channels hosting the alkali cations (Fig. 1). The chains
comprise three crystallographically independent Ti-
atoms in their translation period, all in distorted octa-
hedral chalcogen coordinations. The TiTe6-octahedra
˚
Te bond distances (2.960(2) and 3.025(2) A) within
the pairs are distinctly larger than expected for a Te–
˚
Te single bond (r(Te)cov = 1.39 A).
In K4Ti3Te9 the four crystallographically inde-
share opposite faces, however, due to the deformation pendent alkali-cations occupy the triangular channels
of the octahedra the resulting arrangement is not a lin- formed by the packing. As might be expected, each of
ear but a slightly ondulated chain with Ti-Ti-Ti an- them connects three anionic chains. Due to their off
gles close to 166◦ (see Table 3). The Ti-Ti distances centred positions and due to the severe distortions of
˚
are close to 3.0 A virtually ruling out any homonu- the TiTe6 octahedra their chalcogen environments are
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A. Kolb – K. O. Klepp · K4Ti3Te9
637
irregular. K(1) and K(3) are both in distorted mono-
Partial Te-Te bonds are well established in com-
capped trigonal prismatic coordinations (Fig. 3). The pounds containing hypervalent tellurium [24] in
trigonal prisms are connected via common edges to square planar (pseudo octahedral) coordination by its
build infinite corrugated chains running along [010] homonuclear neighbour leading to the formation of
which in turn are connected via the ditelluride pairs discrete Te65− groups as for instance in Ga2Te5 [25],
yielding a layered arrangement. No proper rationaliza- K2SnTe5 [26] or Re2Te5 [27], or polymerisation
tion is possible describing the coordinations of K(2) products thereof as in the infinite chains, 1 (Te5)2−
,
∞
or K(4) (seven and nine Te-neighbours, respectively). of Rb2Te5 [28] or Cs2Te5 [29]. The Te-Te distances
˚
Average K-Te distances are calculated as 3.644(6) A.
originating from the hypervalent centre are typically
˚
The most striking feature of the present compoundis in the range of 2.90 – 3.03 A. As has been stated in the
certainly the presences of Te-Te pairs with exception- introduction, similar Te-Te distances (but no square
ally long bond distances. The application of Pauling’s Te5-groups) are found in many alkali polytelluromet-
bond order – bond length relationship [23]
allates of the group IVa-metals but no attempt has
so far been made to reach a rational interpretation of
their occurrence. Since they show a wider spread of
homonuclear bond distances, such an interpretation
appears less obvious and probably would require
extensive theoretical calculations, in particular for
tellurium-rich compounds like K4Hf3Te17 [18] where
the system of partial Te-Te bonds extends over several
tellurium atoms. For K4Ti3Te9 it should be easier
since only tellurium pairs need to be considered.
Conductivity measurements and the determination of
the magnetic susceptibility should, in addition, help
dn = d1 −0.71log n
reveals fractional bond orders of 0.55 and 0.45 for
˚
d1 = 2.78 A which comes close to 0.5. The reduc-
tion of the bond order with respect to that of a “nor-
mal” ditelluride (Te22−) group could be explained by
the presence of one further electron occupying an anti-
bonding level of the ditelluride unit yielding Te32−. Ne-
glecting weak bonding interactions between the ditel-
luride groups and their tellurium neighbours (the near-
est homonuclear neighbours of the two pairs are at
to clarify the bonding situation within the [Ti3Te9]4−
anions.
-
˚
3.215(2) and 3.333(2) A apart) the Te2-units might
be considered as isolated groups. Under this assump-
tion the crystal chemical formula can be rationalized
as (K+)41∞[(Ti4+)3(Te2)3−2(Te2−)5]. In the normal va-
lence compound Tl2TiTe3 [22] which – for easier com-
parison – may be formulated as Tl6Ti3Te9 a sufficient
number of electrons can be supplied by the cations and
homonuclear Te-Te bonding is no longer necessary.
Acknowkedgement
Financial support of this work through the Jubila¨ums-
¨
fonds der Osterreichischen Nationalbank (project no. P6427)
is gratefully acknowledged.
[1] K. O. Klepp, Z. Naturforsch. 40b, 229 (1985).
[2] C. Rumpf, W. Bensch, Z. Naturforsch. 55b, 695
(2000).
[3] R. Tillinski, C. Na¨ther, W. Bensch, Z. Kristallogr.
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