Synthesis and structure determination of In3TeO 3F7: An indium oxyfluorotellurate IV derived from W bronze structure with Te4+ in hexagonal tunnels

Article abstract of DOI:10.1016/j.jallcom.2010.10.139

After InTeO₃F and InTe₂O₅F recently described, a new compound In₃TeO₃F₇ is characterized in the In-Te^IV-O-F system. The crystal structure was determined by single X-ray diffraction and refined to R₁ = 0.028. In₃TeO₃F₇ crystallizes in orthorhombic space group Cmmm, a = 7.850(2) , b = 27.637(6) , c = 4.098(1) , V = 889.1(4) ³ and Z = 4. Its structure consists of the stacking, via vertices, of identical layers composed of InF₆ and InO₂F₄ octahedra sharing corners and of InO₄F₃ pentagonal bipyramids sharing edges and vertices. The Te cations statistically occupy one or the other of two close sites located inside tunnels delimited by the In polyhedra and are bonded to F anions located in the same tunnels. The structure can be considered as an intergrowth of parallel strips of MIn₃F ₁₀ and hexagonal tungsten bronze (c)-types. It is compared to other structures such as the bronze Sb_0.157WO₃, TeMo ₅O₁₆ and Sb₂Mo₁₀O₃₁, phases also comprising Te⁴⁺ or Sb³⁺ inside hexagonal tunnels. The electronic lone pair of Te⁴⁺ is stereochemically active and a perfect O/F ordering occurs on the anionic sites.

Full text of DOI:10.1016/j.jallcom.2010.10.139

Journal of Alloys and Compounds 509 (2011) 1517–1522
Contents lists available at ScienceDirect
Journal of Alloys and Compounds
journal homepage: www.elsevier.com/locate/jallcom
Synthesis and structure determination of In3TeO3F7: An indium
oxyfluorotellurate IV derived from W bronze structure with Te4+ in
hexagonal tunnels
N. Jennene Boukharrata∗, J.P. Laval
Laboratory of «Science des Procédés Céramiques et de Traitements de Surface», UMR-CNRS n◦ 6638, Limoges University, 123, Avenue A. Thomas, 87060 Limoges Cedex, France
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 8 July 2010
Received in revised form 17 October 2010
Accepted 27 October 2010
Available online 2 November 2010
After InTeO3F and InTe2O5F recently described, a new compound In3TeO3F7 is characterized in the
In–TeIV–O–F system. The crystal structure was determined by single X-ray diffraction and refined to
˚
˚
R1 = 0.028. In3TeO3F7 crystallizes in orthorhombic space group Cmmm, a = 7.850(2) A, b = 27.637(6) A,
3
˚
˚
c = 4.098(1) A, V = 889.1(4) A and Z = 4. Its structure consists of the stacking, via vertices, of identical lay-
ers composed of InF6 and InO2F4 octahedra sharing corners and of InO4F3 pentagonal bipyramids sharing
edges and vertices. The Te cations statistically occupy one or the other of two close sites located inside
tunnels delimited by the In polyhedra and are bonded to F anions located in the same tunnels.
The structure can be considered as an intergrowth of parallel strips of MIn3F10 and hexagonal tung-
sten bronze (c)-types. It is compared to other structures such as the bronze Sb0.157WO3, TeMo5O16 and
Sb2Mo10O31, phases also comprising Te4+ or Sb3+ inside hexagonal tunnels. The electronic lone pair of
Te4+ is stereochemically active and a perfect O/F ordering occurs on the anionic sites.
© 2010 Elsevier B.V. All rights reserved.
Keywords:
Indium tellurium IV oxyfluoride
Crystal structure
Bronze structure
MIn3F10 structure
Oxyfluorotellurate
Disorder
1. Introduction
2. Experimental methods
In recent years, a systematic investigation of oxyfluorotellu-
rates(IV) has been started, in order to extend the field of materials
likely to present interesting optical non-linear properties, reserved
to oxides until now. Introducing an extra anion as F−, acting as a
modifier of tellurates IV environment, successively, new oxyflu-
orides, TeOF2 [1] and Te2O3F2 [2], oxyfluorotellurates: MTeO3F
(M = Fe, Cr, Ga, In, Sc) [3,4], V2Te2O7F2 [5], TiTeO3F2 [5] and
InTe2O5F [6] have been synthesized and structurally characterized.
In these last phases, the trivalent or tetravalent cation associated
to tellurium IV is in octahedral coordination. Some of them being
non-centrosymmetric, their Second Harmonic Generations (SHG)
were studied.
The present work deals with another oxyfluorotellurate (IV):
In3TeO3F7, poorer in tellurium, and presenting different structural
features from the previous phases, with Te4+ inserted inside tun-
nels. It is compared to a few numbers of phases of similar nature
which can be gathered in a homogeneous structural family deriving
from bronze type.
2.1. Crystal synthesis
In3TeO3F7 is obtained as a pure phase by a solid-state reaction
using a mixture of 64 (mol%) InF3–9 (mol%) In2O3–27 (mol%) TeO2
heated in a platinum sealed tube. The composition seems strictly
stoichiometric. However the single crystals used for this study are
obtained from a slightly different composition: 71 (mol%) InF3–29
(mol%) TeO2. The refined lattice parameters are exactly the same
as for the nominal composition.
InF3 and In2O3 were commercial products (Aldrich, 99.9%).
TeO2 was prepared in the laboratory by decomposition at 823 K
under flowing oxygen of commercial H6TeO6 (Aldrich, 99.9%). This
process gives tellurium dioxide of a good quality and reactivity,
without traces of moisture.
To obtain In3TeO3F7 single crystals the following heat treat-
ment is adopted: the temperature was progressively increased to
963 K (5◦ min−1), held for 4 days, then slowly decreased to 693 K
(0.1◦ min−1) and held for 2 days at this last temperature. Finally, the
platinum tube was water-quenched to room temperature. Colour-
less and moisture-resistant tablets were obtained, grown in a more
or less melted mixture. Many were twinned or cleaved. A second
heat treatment was necessary: the product was crushed and heated
a new time in a gold sealed tube. The temperature was progressively
increased to 693 K (5◦ min−1), held for 2 days and then decreased to
∗
Corresponding author. Tel.: +33 0668264231; fax: +33 0555457586.
E-mail address: nefla.boukharrata@unilim.fr (N. Jennene Boukharrata).
0925-8388/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jallcom.2010.10.139

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N. Jennene Boukharrata, J.P. Laval / Journal of Alloys and Compounds 509 (2011) 1517–1522
Table 1
Table 3
Crystal and structure refinement data.
Anisotropic displacement factors (Å2) for In3TeO3F7.
Formula
In3TeO3F7
Atoms U11
U22
U33
U23
U13
U12
0.0000
Formula weight (g)
Temperature (K)
Crystal system
a (Å)
653.05
293
Orthorhombic, Cmmm
7.850(2)
27.637(6)
4.098(1)
889.1(4)
4
In1
In2
In3
Te1
O2
F1
0.0071(4)
0.0059(5)
0.0120(5)
0.0096(4)
0.0088(4)
0.0120(4)
0.0073(4)
0.0064(4)
0.0099(5)
0.0000 0.0000
0.0000 0.0000
0.0000 0.0000 −0.0013(3)
0.0000
0.0091(11) 0.0087(13) 0.0423(11) 0.0000 0.0000 −0.0019(8)
0.008(4)
0.028(5)
0.053(6)
0.033(4)
0.013(4)
0.002(5)
0.023(3)
0.015(4)
0.039(4)
0.037(5)
0.043(4)
0.021(4)
0.056(7)
0.015(2)
0.082(9)
0.010(4)
0.010(4)
0.006(3)
0.065(6)
0.038(7)
0.045(4)
0.0000 0.0000
0.0000 0.0000
0.0000 0.0000
0.0000 0.0000
0.0000 0.0000
0.0000 0.0000
0.0000
0.0000
0.001(4)
0.0000
0.0000
0.0000
b (Å)
c (Å)
Volume (Å3)
Z
F2
F3
F4
F5
dcalc (g cm−3
)
4.879
11.03
1144
ꢀ (mm−1
F(0 0 0)
)
F6
0.0000 0.0000 −0.011(2)
Crystal size (mm)
0.09 × 0.05 × 0.03
ꢁ range (◦)
5.19–27.47
Data collected
−9 < h < 10, −35 < k < 35, −5 < l < 5
5970/634
terns perpendicular to the main axes show the presence of a strong
and well defined orthorhombic C sublattice and of diffuse spots
(Fig. 1) intercalated between the 1kl, 2kl and 3kl reciprocal planes of
the sublattice and forming new 1.5kl, 2.5kl and 3.5kl diffuse planes.
In these planes, the diffuse spots extend along [0 k 0] forming series
of dashed lines, as shown in the representation of the 1.5kl recip-
rocal plane in Fig. 2. Similar observations have been made in many
phases deriving from bronze-like types and generally result from
short or medium range organisation of defects (interstitial cations)
in tunnels. Considering the relative independence of the sublattice,
the diffuse superstructure and also the great difficulty to define
a plausible lattice parameter for the superlattice along [0 k 0], the
present work consists in refining and describing the well-defined
Reflection collected/unique
Refinement method
Data/restraints/parameters
Goodness of fit on F2
Final R indices [I > 2ꢂ(I)]
R indices (all data)
Full-matrix least-squares on F2
634/0/61
1.216
R1 = 0.028, wR2 = 0.053
R1 = 0.045, wR2 = 0.058
2.15 and −1.09
−3
˚
Largest diff. peak and hole (e A
)
593 K (0.1◦ min−1) and held for 4 days at this last temperature. Sim-
ilar colourless tablets were obtained. They were suitable for X-ray
diffraction study.
2.2. Structure solution and refinement
A single crystal of In3TeO3F7 was selected, mounted on a tapered
fibreglass, and placed on a Nonius Kappa CCD four circle diffrac-
tometer. Full space data were collected at room temperature using
monochromatic MoK˛ radiation. Unit cell parameters were refined
using DIRAX/LSQ [7] and data integrated with EVALCCD [8] pro-
grams.
The integrated intensities were corrected for absorption effects
by using a multi-scan method: SADABS [9], lowering Rint from 0.088
to 0.042. Selected data collection parameters and crystallographic
data are provided in Table 1.
The structure was solved by direct methods and refined on the
basis of F2 for all unique data using SHELXS97 [10] and SHELXL97
[10]. The refined atomic coordinates and anisotropic thermal
parameters are listed in Tables 2 and 3 respectively. The selected
interatomic distances for In3TeO3F7 are given in Table 4.
The preliminary study of the diffraction pattern shows that
some anomalies (cleavage, twinning, . . .) occur on most single crys-
tals, whatever the thermal treatment is. Only slight improvements
result from longer time or multiple annealing. The precession pat-
Table 4
Selected interatomic distances (Å) for In3TeO3F7.
In1–O1ii
In1–O1
In1–F3iii
In1–F3
In1–F6ii
In1–F6
2.045(6)
2.045(6)
2.052(1)
2.052(1)
2.095(5)
2.095(5)
In3–F6vi
In3–F6
In3–F4vi
In3–F4
In3–F2iii
In3–F2
2.044(4)
2.044(4)
2.047(2)
2.047(2)
2.0490(5)
2.0490(5)
In2–F1iii
In2–F1
In2–F5
2.051(1)
2.051(1)
2.082(1)
2.184(5)
2.184(5)
2.209(5)
2.209(5)
Te1–O2
Te1–O1
Te1–F7
Te1–F6
Te1–O1i
1.810(9)
2.023(6)
2.065(3)
2.853(7)
2.864(7)
In2–O2v
In2–O2
In2–O1iv
In2–O1
(i) − x + 2, y, −z; (ii) − x + 1, y, −z; (iii) x, y, z − 1; (iv) x, −y +
1, −z; (v) − x + 2, −y + 1, z; (vi) − x + 32 , −y + 23 , z.
Table 2
Atomic coordinates and equivalent isotropic displacement factors Ueq (Å2) for
In3TeO3F7.
Atoms
x
y
z
Ueq
In1
In2
In3
Te1
Te2
O1
O2
F1
F2
F3
F4
F5
0.5000
0.7652(1)
0.7500
0.9434(4)
0.9032(19)
0.7051(7)
1.000
0.7541(9)
0.7500
0.5000
1.0000
0.5000
0.6846(7)
0.929(3)
1.0000
0.6237(1)
0.5000
0.7500
0.6059(1)
0.6225(7)
0.5781(2)
0.5424(3)
0.5000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.5000
0.5000
0.5000
0.0000
0.0000
0.0000
0.5000
0.5000
0.0080(2)
0.0070(3)
0.0113(3)
0.0200(7)
0.023(3)
0.0163(12)
0.035(3)
0.0257(19)
0.034(2)
0.0271(17)
0.033(2)
0.032(3)
0.0276(13)
0.005(5)
0.005(5)
0.7500
0.6275(3)
0.7290(3)
0.5000
0.6784(1)
0.6143(8)
0.5962(17)
F6
F7
F8
Fig. 1. hk0 reciprocal plane of the sublattice.

N. Jennene Boukharrata, J.P. Laval / Journal of Alloys and Compounds 509 (2011) 1517–1522
1519
Fig. 2. 1.5kl reciprocal diffuse plane showing the dashed lines of diffuse spots.
Fig. 4. Projection onto (0 0 1) plane of the two dimensional network of In polyhedra
with Te cations occupying the tunnels.
substructure and trying to determine, as well as possible, a defect
model able to explain the main features of the superstructure.
bronze (HTB) layer. This last structure is formed by the stacking
of six corner-shared WO6 octahedra enclosing an hexagonal tun-
nel which can be occupied by an extra cation. In In3TeO3F7, two
of the six octahedra are replaced by two pentagonal bipyramids
sharing an edge (Fig. 4). The angles In1–F6–In3 = 150.9(5)◦ and
In3–F4–In3 = 146.6(7)◦ are comparable to W–O–W = 150◦ [14].
The strips of both substructures alternate by sharing vertices
along [0 1 0] to give a host framework enclosing one-dimensional
tunnels of almost hexagonal section (Fig. 4). The In3TeO3F7 struc-
ture can then be considered as resulting from the intergrowth
of MIn3F10 and HTB structures. The indium cations form a mixed
[(3.6.3.6)2.(32.62)] plane net associating two types of regular plane
nets: 3.6.3.6 and 32.62 [15].
The tellurium cations are inserted inside these tunnels and are
delocalized from their centre towards the side occupied by oxygen
atoms. This phenomenon can be explained by the activity of the
lone pair E of tellurium IV and is also observed in the MTeF5 (M = K+,
Na+, Rb+, Cs+, Tl+ and NH4+) [16] phases in which tellurium atoms
are not in the centre of anionic cubes but shifted towards one of the
square faces.
3. Results and discussion
3.1. Basic structure description
In the In3TeO3F7 structure, indium cations are in six- and seven-
fold coordination, in agreement with the crystal chemistry of this
trivalent cation, e.g. in MIn3F10 series (M = Rb, Cs, Tl, NH4) [11] and
Ba5In3F19 [12].
The In13+cation is surrounded by four fluoride and two oxygen
atoms forming an almost perfect InO2F4 octahedron (Fig. 3a). Each
In23+ cation forms an InO4F3 pentagonal bipyramid (Fig. 3b). The
In33+ ion occupies the centre of an almost perfect InF6 octahedron
(Fig. 3c). The main interatomic distances are given in Table 4.
Two basic units can be distinguished in this structure and refer
to two different structural types. The first consists of the association
of four polyhedra: two In2O4F3 pentagonal bipyramids linked by F5
vertices and sharing O1 corners with two In1O2F4 octahedra. These
units share (O2–O2) edges to form strips parallel to [1 0 0] (Fig. 4).
Similar strips constitute the basis of the MIn3F10 and NaMIIZr2F11
[13] structures.
In In3TeO3F7 structure, the tellurium site is very close to a mirror
˚
plane so that its symmetric site is at only 0.888 A. The two sites have
The second unit consists of chains of In3F6 tilted octahedra shar-
ing F4 corners along [1 0 0]. Associated to the first basic units along
[0 1 0] (Fig. 4), they constitute the 2/3 of an hexagonal tungsten
the same energy and the same anionic environment but cannot be
occupied simultaneously. The Te1 cations and, by extension, the
hexagonal tunnels form a semi-regular 33.42 plane net [15], inter-
Fig. 3. Anionic polyhedra of: (a) In13+ [symmetry codes: (ii) −x+1, y, −z; (iii) x, y, z − 1]. (b) In23+ [symmetry codes: (iii) x, y, z − 1; (iv) x, −y + 1, −z; (v) −x + 2, −y + 1, z]. (c)
In33+ [symmetry codes: (iii) x, y, z − 1; −x + (3/2), (−y + (3/2)), z].

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N. Jennene Boukharrata, J.P. Laval / Journal of Alloys and Compounds 509 (2011) 1517–1522
Fig. 5. Several models of short range order of the atoms Te and F inside the tunnels: (a) the tellurium cations Te1 and the fluoride anion (F7) occupy the sites of the same
side of the mirror. (b) One tellurium and the fluoride atoms occupy the sites of one side of the mirror and the second tellurium occupies the site of the other side. (c) The two
tellurium atoms occupy the sites of the first side of the mirror and the fluoride one occupies the site of the second side. (d) A simplified model of the tellurium atoms inside
the tunnels. [Symmetry codes : (i) − x + 2, y, − z ; (vii) x, y, z + 1 ; (viii) − x + 2, y, − z + 1].
mediate between 36 and 44 triangular and square regular plane
nets respectively.
Table 5
Bond valence calculations for In3TeO3F7.
Atoms
In1
In2
In3
Te1
ꢃij
O1
O2
F1
F2
F3
F4
F5
F6
F7
ꢃij
2 × 0.679
2 × 0.436
2 × 0.467
2 × 0.497
0.883/0.091
1.570
2.09
2.50
0.99
1.00
0.99
1.00
0.91
1.04
1.52
3.2. Short range order of Te1 and F7 in hexagonal tunnels
2 × 0.499
2 × 0.502
2 × 0.506
3.01
Each tellurium atom is strongly bonded to two oxygen atoms
O1 and O2 occupying two vertices of the hexagonal section of
the tunnel and to a fluoride anion F7 inserted in the tunnel. Two
additional anions O1i and F6, occupying two other vertices of the
hexagonal section of the tunnel can be added to the tellurium atom
environment at longer distances (Table 4). The F7 anions and the
Te1 cations statistically occupy two different sites, both close to
2 × 0496
0.456
3.26
2 × 0.441
0.091
0.761
3.40
3.23
˚
the (0 1 0) mirror plane with short distances: F7–F7 = 1.11(5) A and
˚
Te1–Te1 = 0.888(6) A. Therefore, Te1 site is half-occupied but F7 one
is only quarter-occupied. Then, there is only one F7 anion available
for two Te1 cations, which is necessarily located between these two
cations. Considering the splitting of the Te1 and F7 sites, several
models of short range order can be imagined, from the statistical
structure, to describe the local structure inside the tunnels. The
[Te2O4F]− bipolyhedra can be linear or angulated. The linear ones
are lined up parallel to [0 0 1] and occupy one or the other side of
the mirror plane (Fig. 5a) and the angulated ones with Te1 and/or
F7 atoms occupy both sides of the mirror plane (Fig. 5b and c). How-
ever, the most probable arrangement consists of linear bipolyhedra
occupying in a disordered way one side or the other of the mirror
plane (Fig. 5d). This last model leads to the better agreement in bond
valence calculations (Table 5) and gives more regular Te1 polyhedra
and more logical interatomic distances than the other ones. Sim-
ilar bipolyhedra have already been described in a few number of
bronze-related structures also containing a lone pair cation: Te4+
or Sb3+ inside hexagonal tunnels: Sb0.16WO3 [17], TeMo5O16 [18]
and Sb2Mo10O31 [19].
Fig. 6. Several configurations of cations with lone pairs E inside hexagonal tunnels: (a) comparison between Sb3+ in Sb0.16WO3 an Te4+ in In3TeO3F7; (b and c) connectivity
of Te4+ and Sb3+ inside the tunnels in TeMo5O16 and Sb2Mo10O31 respectively.

N. Jennene Boukharrata, J.P. Laval / Journal of Alloys and Compounds 509 (2011) 1517–1522
1521
The structure of Sb0.16WO3 is an intergrowth tungsten bronze
(ITB) characterized by parallel slabs of HTB and perovskite types.
Inside the hexagonal tunnel, the Sb3+ cation occupies the same
position as Te4+ in In3TeO3F7, split over two sites symmetrically
shifted from the centre of the tunnel on each side of the mirror
plane (Fig. 6a). A complex superstructure has also been revealed,
qualitatively explained by a partially ordered distribution of the
Sb3+ cations on these split sites.
TeMo5O16 (orthorhombic variety) and Sb2Mo10O31 structures
are also based on quite similar ITB planes but with a filling of the
hexagonal tunnels by [Te–O] and [E–Sb–O–Sb–E] chains respec-
tively (Fig. 6b and c). This last configuration corresponds to the
first short range order model proposed in Fig. 5a for Te1 and F7 in
a linear [Te2O4F]− bipolyhedron.
At this stage of −th3 e refinement, some residual electronic den-
sity (ꢄꢅ1 = 5.62 e A and ꢄꢅ2 = 2.91 e A−3) remains near Te1 and
˚
˚
˚
˚
F7 sites respectively. The first peak is at 1.98 A from O1 and 2.02 A
˚
˚
from F6. The second is at 2.16 A and 2.44 A from Te1 and O2 respec-
tively. These distances are in agreement with theoretical ones.
In these conditions, R1 = 0.046 and wR2 = 0.100. The treatment of
these residual electronic densities as extra Te2 and F8 sites respec-
tively gives: R1 = 0.028 and wR2 = 0.058 with much lower residues
of electronic density (ꢄꢅmax = 2.15 e A−3 and ꢄꢅmin = −1.09 e A−3).
The presence of these Te2 and F8 sites, weakly occupied, can
likely be explained by more complex chain associations of Te poly-
hedra as proposed in Fig. 5, in which a slight shift of Te1 and F7 sites
in respectively Te2 and F8 ones should occur. The final refinement
has taken into account this hypothesis in correlating the occupancy
rate of the mutually incompatible Te1–Te2 and F7–F8 sites in order
to obtain a full occupancy for the sum of their respective amount.
˚
˚
Fig. 7. Schematic representation of tellurium atoms (blue circle) ordering along
[1 0 0] and [0 1 0] directions. White circles show the unoccupied tellurium sites in
this model. (For interpretation of the references to colour in this figure legend, the
reader is referred to the web version of the article.)
between the closest Te1 bipolyhedra along [0 1 0] but much looser
between the more distant ones. This hypothesis must, of course, be
verified by more thorough calculations, made difficult by the resid-
ual disorder corresponding to the Te2 and F8 components of the Te1
and F7 sites in the tunnels. Similar superstructures are described in
Sb0.16WO3 but not yet fully explained.
3.3. O/F order
The bond valences are calculated by the Brown’s method [20]
and illustrated in Table 5. A perfect O/F ordering is present on the
anionic sites. It is well correlated to the position of the Te1(Te2)
cations. Indeed, these last atoms are systematically closer to the
three O anions and conversely farer from the three F ones compos-
ing the six vertices of the hexagonal tunnel section at the same z
level. As each Te1 cation is strongly bonded to two of these three
O anions, two equivalent positions are possible for each Te1 cation
as above discussed.
4. Conclusion
In conclusion, this new structure type is particularly interesting
by the presence of Te4+ inside the tunnels of an hybrid structure
of HTB and MIn3F10 types. A partial ordering of the Te1 polyhedra
located inside the tunnels tentatively explains the intense diffuse
scattering observed. It should be interesting to approach more
quantitatively the structural features of this diffuse superstruc-
ture and to try to synthesize other compounds containing lone pair
cations inside cavities of such structures.
3.4. Diffuse superstructure: models of medium range order
Considering that the a parameter is unambiguously doubled,
after the diffuse superlattice planes (see Section 2) and that the
Cmmm space group is likely unchanged in the superlattice, half
mirror planes perpendicular to [1 0 0] disappear, letting virtually
unchanged the In skeleton but not the Te1(Te2) and F7(F8) frame-
work. The main cause for the existence of a superlattice is likely the
loss of the statistical character of Te1 and F7 positions which in the
superlattice are likely long range ordered along [1 0 0] direction.
Fig. 7 shows how, in a row of hexagonal tunnels along the [1 0 0]
direction, the successive shift of [Te2O4F]− bipolyhedra leads to a
doubling of the a parameter, using the Cmmm space group. The
presence of extensive diffusion of the spots along [0 1 0] (Fig. 2)
can be rationalized in the following way: if the Te1–Te1 distances
are relatively long and regular along [1 0 0], extending from 6.90 to
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in
the online version, at doi:10.1016/j.jallcom.2010.10.139.
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˚
8.91 A, two different kinds of Te1–Te1 distances are present along
[0 1 0], long ones for which two Te1 cations are separated by a In3F6
˚
˚
octahedron (8.43–9.27 A) and shorter ones (5.94, 6.01 A), for which
these cations are only separated by an O2–O2 edge connecting two
In2F3O4 pentagonal bipyramids (Fig. 7).
The long range ordering between [Te2O4F]− bipolyhedra, more
or less strictly established along [1 0 0], is likely rather strict
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