research papers
Structural transformation of Sbbased highspeed phasechange material
^{a}Device Solutions Center, R&D Division, Panasonic Corporation, 311 YagumoNakamachi, Moriguchi, Osaka 5708501, Japan, ^{b}AVC Networks Company, Panasonic Corporation, 115 Matsuocho, Kadoma, Osaka 5718504, Japan, ^{c}Department of Materials Science & Engineering, Kyoto University, Yoshidahonmachi, Sakyoku, Kyoto 6068501, Japan, ^{d}Graduate School of Science, Osaka Prefecture University, 11 Gakuencho, Sakai, Osaka 5998531, Japan, and ^{e}Faculty of Liberal Arts and Sciences, Osaka Prefecture University, 11 Gakuencho, Sakai, Osaka 5998531, Japan
^{*}Correspondence email: matsunaga.toshiyuki@jp.panasonic.com
The _{3.4}In_{3.7}Sb_{76.4}Te_{16.5}) enclosed in a vacuum capillary tube was investigated at various temperatures in a heating process using a large Debye–Scherrer camera installed in BL02B2 at SPring8. The amorphous phase of this material turns into a crystalline phase at around 416 K; this crystalline phase has an A7type structure with atoms of Ag, In, Sb or Te randomly occupying the 6c site in the This structure was maintained up to around 545 K as a single phase, although of the crystal was observed. However, above this temperature, into AgInTe_{2} and Sb–Te transpired. The first fragment, AgInTe_{2}, reliably maintained its up to the melting temperature. On the other hand, the atomic configuration of the Sb–Te gradually varied with increasing temperature. This gradual structural transformation can be described as a continuous growth of the modulation period γ.
of a phasechange recording material (the compound AgKeywords: chalcogenide compounds; homologous structure; modulated layer structure; phase change; AIST.
BIncStrDB reference: 6732EXfQbW
1. Introduction
Phase change recording is now extensively used for highdensity nonvolatile memories (Wuttig & Yamada, 2007). Since the 1970s, various materials have been proposed for this purpose, and today we have obtained two superior materials: GeTe–Sb_{2}Te_{3} (GST) (Yamada et al., 1991) and Sb–Tebased alloys such as Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5} (AIST or silver indium antimony tellurium; Iwasaki et al., 1992); these materials are now practically used as the memory layers in phasechange optical disk media, as well as in the memory cells of solidstate electrical memories. Recording can be achieved using laser irradiation or ohmic heating to cause reversible phase changes between the amorphous and crystalline phases. We analyzed the of AIST about 10 years ago (Matsunaga et al., 2001), revealing that AIST has an A7type structure, the same as that of pure Sb, in which four elements randomly occupy the 6c site in the It has been presumed that this simple and spatially isotropic p–p connected sixcoordination structure enables instantaneous transformation from the amorphous phase to the crystalline phase by minimal atomic rearrangement (Matsunaga et al., 2006; Matsunaga, Yamada et al., 2011). Our analysis also revealed that this A7type quaternary crystal held its rhombohedral structure, showing a continuous atomic shift along the axis from z = 0.233 to 1/4, when the temperature was raised close to the melting point. We examined the crystal structures of Sb–Te binary compounds, which are the mother alloys of the AIST materials, as well as those of Bi–Te compounds. These compounds are known, in thermal equilibrium, to have a series of commensurately or incommensurately modulated longperiod layer structures, depending on their binary compositions, between Sb and Sb_{2}Te_{3} or between Bi and Bi_{2}Te_{3}. Our present investigation of an asdeposited Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5} amorphous film in a sealed quartz tube revealed that when the temperature was raised, this quaternary alloy maintained an A7type structure, hardly showing any atomic shift. However, decomposition into two phases, AgInTe_{2} and Sb–Te, occurred at around 545 K. After this decomposition, the atomic configuration of the Sb–Te fragment with the A7type disordered structure gradually moved into an ordered arrangement to finally obtain a stable homologous structure ruled by its composition. This can be considered as follows: the dopants, Ag and In, played roles in simplifying the structure of the quaternary alloy. However, once these dopants were lost, the structural feature of the Sb–Te binary compound revealed itself.
2. Experimental
A thin film of Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5} with a thickness of approximately 300 nm was formed by sputtering on a glass disk 120 mm in diameter. The film was scraped off with a spatula to create a powder, which was then packed into a quartz capillary tube with an internal diameter of 0.3 mm. To prevent it from reacting with components of air, we sealed the opening of the capillary tube using an oxyacetylene flame. The diffraction experiments were carried out using the largediameter Debye–Scherrer camera with an imaging plate on the BL02B2 beamline at the Japan Synchrotron Radiation Research Institute (Nishibori et al., 2001). The energy of the incident beam was approximately 29.4 keV. An imaging plate with a pixel area of 100 µm^{2} was used as the detector; this pixel area corresponded to an angular resolution of 0.02° (287 mm camera diameter). However, for more precise structure analyses, intensity data in increments of 0.01° were obtained by reading the imaging plate for a pixel area of 50 µm^{2}. Experiments at low and high temperatures were carried out while blowing nitrogen gas onto the capillary tube at the specified temperatures. The crystal structures were examined and refined using the (Rietveld, 1969); the programs JANA2000 (Petříček & Dušek, 2000) and JANA2006 (Petříček et al., 2006) were used for this purpose. The energy of the synchrotron radiation was confirmed by recording the diffraction intensity of CeO_{2} (a = 5.4111 Å) powder as a reference specimen at room temperature under the same conditions, which showed that the wavelength used for the structural analyses was 0.4187 (3) Å. Neutral atomic scattering factors were employed for them.
3. Results and discussion
3.1. Crystals observed in this experiment
The diffraction patterns obtained for the sputtered Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5} amorphous film are shown in Fig. 1. The amorphous phase transformed into an A7type crystalline single phase, as seen in this graph, at around 416 K. The results of a search match and Rietveld analyses revealed the diffraction patterns taken from 435 to 545 K to be almost identical to that of an As, Sb or Bi crystal with an A7type structure (Clark, 1955), as has been previously elucidated (Matsunaga et al., 2001). The (conventional threedimensional) Rietveld analysis results at 545 K are shown in Table 1(a). This crystal belongs to the ; the four constituent elements, Ag, In, Sb and Te, randomly occupy the 6c site (Matsunaga, Akola et al., 2011). The changes in the diffraction lines with increasing temperature show that the singlephase A7type structure is maintained up to around 545 K. However, the peaks for CuFeS_{2}type AgInTe_{2} (Wyckoff, 1986) appear at around 590 K, along with those of the A7type structure. This decomposition can be written as
These two phases formed by heating coexisted up to the high temperatures at which their Bragg peaks almost disappeared as a result of dissolving. As seen in this equation, the second decomposition product can virtually be regarded as an Sb–Te binary compound. Even at high temperatures close to the melting temperature, AgInTe_{2} tightly held the CuFeS_{2}type structure irrespective of temperature. However, our present analysis revealed that the structure of the second fragment, the Sb–Te compound, gradually changed with increasing temperature until obtaining its final stable atomic configuration. These structures can be closely approximated by the A7type structure but are not real A7type ones.
3.2. Homologous structures
We examined many types of chalcogenide materials to clarify the highspeed phasechange mechanism and develop new materials for future ultrahighdensity phasechange recording devices. This revealed that, after sufficient heat treatments, almost all these materials finally fell into their stable crystals with socalled homologous structures. It has been found that in thermal equilibrium, the typical phasechange materials, the GeTe–Sb_{2}Te_{3} pseudobinary system, the Sb–Te or Bi–Te binary system, form various intermetallic compounds represented by the chemical formulae (GeTe)_{n}(Sb_{2}Te_{3})_{m}, (Sb_{2})_{n}(Sb_{2}Te_{3})_{m} or (Bi_{2})_{n}(Bi_{2}Te_{3})_{m} (n, m: integer). All these compounds have trigonal structures with 2n + 5m cubic closepacked periodicity (almost) without exception. [More specifically, the residual of (2n + 5m)/3 = 0 and ≠ 0 leads to the formation of crystals having structures with primitive (P) and rhombohedral (R) unit cells; they form structures with N = (2n + 5m) and N = 3*(2n + 5m) layers, respectively.] Table 2 shows the case of the GeTe–Sb_{2}Te_{3} compounds; all of the existing intermetallic compounds in these systems follow this rule (Matsunaga & Yamada, 2004a; Matsunaga, Yamada & Kubota, 2004; Matsunaga et al., 2007a,b, 2010; Matsunaga, Kojima et al., 2008). This could also be confirmed from the relevant tables in other papers (Karpinsky et al., 1998; Kuznetsova et al., 2000; Shelimova et al., 2000, 2004; Shelimova, Karpinskii et al., 2001; Shelimova, Konstantinov et al., 2001; Poudeu & Kanatzidis, 2005). These structures are similar to each other and systematically characterized by the stacking of the (GeTe)_{n} and (Sb_{2}Te_{3})_{m}, (Sb_{2})_{n} and (Sb_{2}Te_{3})_{m}, or (Bi_{2})_{n} and (Bi_{2}Te_{3})_{m} blocks along the axes, with very long cell dimensions in the conventional threedimensional structure description (Karpinsky et al., 1998; Shelimova et al., 2000; Shelimova, Karpinskii et al., 2001; Poudeu & Kanatzidis, 2005; Matsunaga & Yamada, 2004a, Matsunaga, Yamada & Kubota, 2004; Matsunaga et al., 2007a,b, 2010; Matsunaga, Kojima et al., 2008; Matsunaga, Morita et al., 2008). More generally and more precisely it has been assumed that these structures should be described as commensurately or incommensurately modulated fourdimensional structures characterized by modulation vectors (Lind & Lidin, 2003), where γ values are real numbers equal to or around 3(n + 3m)/(2n + 5m) [see equation (3); is the fundamental reciprocal vector formed by threelayer cubic stacking]. For instance, it has been clarified that, in the thermal equilibrium, Sb_{8}Te_{3} (n = 3 and m = 1) has a homologous structure characterized by a modulation vector (Kifune et al., 2005, 2011). Thus, we applied this more universal fourdimensional method for analysis of the Sb–Te compound formed by thermal decomposition [see equation (1)].

3.3. Structures of Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5} and Sb_{89}Te_{11} compounds
As the initial structure models for the fourdimensional Rietveld refinements we adopted the layer stacking structures defined by the respective γ values. In other words, in the Sb–Te compounds examined in this study, the modulation functions for Sb and Te atoms were respectively distributed around t = 0 and t = 1/2 (t: internal parameter along the x_{4} axis, the fourth crystal axis in fourdimensional space; Lind & Lidin, 2003). This corresponds to a structure in which Sb and Te are placed at 0, 0, 0 and their atomic species are distinguished using crenel functions (for Sb_{89}Te_{11}, width: 0.89 + center: 0 for Sb and width: 0.11 + center: 0.5 for Te). As there is a difference of only one between the atomic numbers of Sb^{51} and Te^{52}, it is very difficult for us to distinguish the kinds of atoms in their unit cells. We use the assumption that all of the Sb–Te crystals examined in this study have perfectly ordered atomic arrangements like those of other (binary) systems. The intensities of the satellites for Sb–Te compounds are rather weak in general. Those of Sb_{89}Te_{11} are no exception; almost all of the satellites observed were reproduced by adopting the maximum satellite index of 2 for the Rietveld analyses. The atomic displacements were represented using harmonic functions.
The fourdimensional Rietveld analyses performed with the diffraction patterns in Fig. 1, as mentioned above, provided the structural dependence on the temperature for Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5} (at low temperatures) and its thermally decomposed materials (at high temperatures). The results of the Rietveld analyses at 545 K for Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5}, whose crystal still maintains an A7type structure, are shown in Table 1(b) and Fig. 2 (cf. Table 1a, from the threedimensional Rietveld analysis). In the fourdimensional analysis for this crystal, displacement for only a single atom in a threedimensional has to be described by selecting the appropriate one from among several kinds of modulation functions; in this case, the use of a sawtooth function (Dušek et al., 2010) was revealed to give better results than a harmonic function, as seen in Fourier maps based on F_{o} (Fig. 3). We can see from Fig. 4, γ maintained a constant value of 1.5 up to a temperature of around 590 K, at which AgInTe_{2} came out. However, above this temperature, γ grew larger with increasing temperature and reached a value of around 1.55 at high temperatures near the melting point of Sb_{76.4}Te_{9.7} (= Sb_{88.7}Te_{11.3} when expressed as a percentage), which was found at around 870 K according to our present hightemperature measurement. The γ value was maintained at around 1.55 even when the powder specimen was cooled back to room temperature. The results of the Rietveld analysis at room temperature are shown in Table 3(a) and Fig. 5. The refined modulation functions of Sb and Te and the corresponding de Wolff section of the observed Fourier map are shown in Fig. 6(a), together with a Fourier map based on F_{o}. The difference Fourier maps obtained from the determined structure models exhibited few significant residual peaks, which showed the need for further structural modification or improvement. This was similar to those obtained at the high temperatures of 774 and 820 K. The γ values of around 1.55 found in these stagnated structures correspond well with the value of 1.5565 expected from the composition of Sb_{88.7}Te_{11.3}. Here we can simply derive γ in terms of x as
when the chemical formula for the binary system is written as Sb_{x}Te_{1 − x} or Bi_{x}Te_{1 − x} (Lind & Lidin, 2003). It can be considered that after Sb_{76.4}Te_{9.7} was segregated from AgInTe_{2}, it revealed its original crystalline nature to change the layer period (γ) from 1.5 (n = 1, m = 0; A7type sixlayer structure) to 1.55 (another longperiod layer structure), and it also clarified that, surprisingly enough, even an Sb–Te compound with as much as 89% Sb can exist as a single homologous structure in its binary system. We can obtain
by comparing Sb_{x}Te_{1 − x} with (Sb_{2})_{n}(Sb_{2}Te_{3})_{m}. The (γ ≃ 1.55) at high temperatures at which the γ growth became stagnant can be approximated reasonably well by a commensurately modulated 29layer structure with n = 12 and m = 1 (γ = 45/29; this threedimensional structure model is shown in Fig. 7a). We also carried out a Rietveld analysis assuming that this Sb–Te crystal had a commensurately modulated structure with this rational number of γ. As shown in Table 3(d), this analysis gave almost the same good results as in the incommensurate case (however, for this material it could not be concluded that it had transformed to a commensurate threedimensional structure, in contrast to Sb_{87}Te_{13}, which will be discussed later). The Fourier map obtained from this fourdimensional analysis performed in the commensurate case is almost identical with all those in Fig. 6, as expected. In addition to the γ dependence on temperature of this Sb–Te material, the Sb_{8}Te_{3} sputtered amorphous film showed a small γ value just after the transformation to the crystalline phase. However, γ became larger with increasing temperature to finally obtain its original longperiod layer structure. We found that, in addition to the Sb_{8}Te_{3} film, some other Sb–Te films at various compositions show very similar behavior (we will show the results for these materials elsewhere in the near future). These results strongly suggest that not a few (at least) Sb–Te compounds, just after their crystal formations, transiently assume small γ values (it is highly probable that these γ values all start at 3/2), and when adequately treated with heat, they become larger to attain their respective, intrinsic homologous structures, depending on their binary compositions.

The atomic displacements (modulation functions) have already been shown in a stagnant structure of Sb_{89}Te_{11} (see Fig. 6). However, just after the phase decomposition, the atomic displacements varied appreciably, as seen in Fig. 8. This figure shows, however, that such a varied atomic arrangement becomes more moderate with increasing temperature, and comes closer to those observed in the stagnated structures. In response to this structural change, although the interatomic distances in Sb_{89}Te_{11} just after the phase decomposition are rather dispersed, especially for Te–Sb pairs, they converge with the structural inactivation, as seen in Fig. 9. As mentioned above, before the phase decomposition, Sb and Te atoms (and the dopants) were randomly distributed in the A7type structure. Therefore, it is expected that just after the decomposition, the crystal still has a strongly disordered atomic arrangement. However, during the structural change with increasing temperature, it gradually attains the perfectly ordered structure shown above (Kifune et al., 2011).
As mentioned above, we used harmonic functions to describe the atomic displacements. However, to examine them more precisely, the JANA2006 program provides several other functions in addition to the harmonic one. We performed further analyses by using some of these functions. However, these analyses gave us almost the same results as shown in Fig. 6 and Tables 3(b) and (c).
3.4. Suitability of Sb–Tebased compounds for highspeed phasechange recording devices
As has so far been shown, an Sb–Te compound containing Ag and In maintains a sixlayer structure (γ = 3/2) up to a high temperature, at which occurs. On the other hand, Sb–Te films without such dopants show γ values larger than 3/2 immediately after the crystallization. This strongly suggests that the Ag and In dopants play roles in maintaining the simple structure of the Sb–Te matrix. It also inversely implies that every Sb–Te binarycompound film will experience a sixlayer structure in a very short time right after the crystal formation because six layers is the simplest and shortest layer structure out of all of the possible homologous structures from Sb (γ = 3/2) to Sb_{2}Te_{3} (γ = 9/5). Many studies (for instance, Matsunaga, Akola et al., 2011) have shown that phasechange chalcogenide amorphous materials have spatially isotropic atomic arrangements; it is highly likely that they crystallize once into simple and spatially isotropic structures, like a cubic crystal, because a sixlayer (A7type) structure can be well approximated by simple cubic lattices (Matsunaga & Yamada, 2004b).
The atomic configuration in the amorphous phase of this material, which has already been revealed (Matsunaga, Akola et al., 2011), is highly disordered, similar to that of a liquid, and spatially has a completely isotropic symmetry. However, it has also been revealed that it has 3 + 3 coordination structures even in such a disordered atomic arrangement, as well as that of the crystalline phase: that is, both phases have very similar coordination structures, i.e. locally very similar atomic arrangements (it is well known that an A7type crystal has a 3 + 3 coordination structure; Clark, 1955; Hoffmann, 1988). This is one of the major reasons that this material achieves a sufficiently high phasechange speed by locally minimal bond interchanges. As for the dopants, it has been presumed that either or both Ag and In atoms probably raise the crystallization temperature of the amorphous phase to obtain a sufficient endurance for longterm data preservation. In addition, as mentioned above, they make the atomic arrangement of the crystal simple and spatially isotropic, holding the material in a single phase. It is expected that these are indispensable features for highspeed rewritable data storage media. In the near future, however, the individual roles played by Ag and In in the phase change of this material should be clarified.
3.5. Three or sixlayer structure approximation for Sb–Te compounds
In our previous work (Matsunaga et al., 2001) Sb–Te compounds with small amounts of Ag or In were concluded to hold an A7type structure up to the melting point. However, we must say that these compounds do not have an exact A7type structure but a longperiod modulated structure defined by the binary composition in thermal equilibrium. The A7type (sixlayer) structure is also one of the modulated structures (corresponding to the shortest period one). All the abovementioned modulated structures can be approximated by a (cubic stacked) threelayer structure, which provides the fundamental lines in the diffraction patterns. If atoms at the 6c site are located at z = 1/4 in the A7type structure, it corresponds to the threelayer structure. In the previous temperature measurement, one end of the capillary holding the powder specimen was open to the air, which yielded not a little Sb oxide (Fig. 10). This oxide formed a line of unnecessary Bragg peaks, which hindered us from determining the (weak) satellite peaks identifying the layer period of the structure. Further, at that time, such modulated structures were not familiarly associated with the Sb–Te binary system. All these factors made it difficult for us to discern that these Sb–Tebased alloys can take modulated structures. Thus, in previous work the A7type structure was exclusively applied in the structural analyses, irrespective of the measurement temperature, which provided apparently sufficient results. In addition, in this work the same structural analysis was carried out to confirm the reproducibility of the previous work; we analyzed the structures by applying this simple 6R structure to them. The results are shown in Table 4. As shown in this table, the R factors were sufficiently low and the positional parameter z gradually increased with temperature (which meant that the structure model for the Rietveld analysis gradually became closer to the threelayer structure), which accurately reproduced the previous results. However, the agreement between the profiles of the observed and calculated intensities became worse as the temperature rose, especially for the (weak) satellite reflections. On the other hand, those obtained through the fourdimensional analyses showed good agreement with each other, even at high temperatures near the melting point, as seen in Fig. 10. This strongly indicates that at high temperatures beyond the (or in the thermal equilibrium), this Sb–Te compound is not an A7type structure (γ = 3/2) itself but one of the homologous structures defined by γ > 3/2.

The present examination clarified that this Sb–Te compound has a longperiod modulated structure like that of the aforementioned Sb_{89}Te_{11}. The modulation period γ kept a constant value of almost 1.5 up to a temperature of around 600 K, at which the oxidation of Sb started. However, above this temperature, just as in the Sb_{89}Te_{11} case, γ grew larger with increasing temperature and reached a value of around 1.56 at high temperatures near the melting point (in contrast, in the previous experiment, Bragg peaks corresponding to AgInTe_{2} were hardly observed for some reason). This γ value indicated that the composition of the compound should be ca Sb_{87}Te_{13} [see equation (2)]. Here, we ignore the locations of Ag and In because they are minor elements. We carried out fourdimensional structural analyses for the two cases where this Sb–Te crystal took an incommensurately or commensurately modulated structure. As shown in Table 5 these analyses gave almost the same good results, when γ = 36/23 (n = 9, m = 1; Sb_{87.0}Te_{13.0}) was applied in the commensurate case (this threedimensional structure model is shown in Fig. 7b). However, the results of the commensurate case could be considered somewhat better than those of the incommensurate case (cf. Table 5a with Table 5b1), in contrast to the examination of Sb_{89}Te_{11}. In addition, we can find a clear t_{0} dependence of the R values in the results of the Rietveld analyses performed in the commensurate case (cf. Table 5b1 with Table 5b2). This strongly suggests that this Sb_{87}Te_{13} compound eventually obtained a (probably stable) commensurate structure through rearrangement of the atoms from the A7type atomic configuration after sufficient heat treatment for this material, as observed in the case of Sb_{8}Te_{3} (Kifune et al., 2011). Generally, the determination between the commensurate and incommensurate case seems to be beyond the information contained in our powder data. However, we believe that it is very likely that many of these compounds ultimately obtain commensurate structures after sufficient heat treatment. We intend to conduct further experiments and analyses for these materials to reveal their structural features more precisely.

4. Conclusions
An Ag_{3.4}In_{3.7}Sb_{76.4}Te_{16.5} quaternary amorphous film was first crystallized into an A7type structure, in which the four types of atoms randomly occupied the atomic sites, right after the phase transformation. However, as the temperature was raised, this single crystalline phase separated into two crystalline phases, AgInTe_{2} and an Sb–Te binary compound. Of these two crystals, AgInTe_{2} was stable up to the melting point. In contrast, the latter crystal, Sb_{89}Te_{11}, had a modulated layer structure, and its modulation vector grew with an increasing in temperature.
Supporting information
BIncStrDB reference: 6732EXfQbW
10.1107/S0108768112039961/dk5006sup1.cif
contains datablocks global, I, II, III, IV, V. DOI:Rietveld powder data: contains datablock I. DOI: 10.1107/S0108768112039961/dk5006Isup2.rtv
Rietveld powder data: contains datablock II. DOI: 10.1107/S0108768112039961/dk5006IIsup3.rtv
Rietveld powder data: contains datablock III. DOI: 10.1107/S0108768112039961/dk5006IIIsup4.rtv
Rietveld powder data: contains datablock IV. DOI: 10.1107/S0108768112039961/dk5006IVsup5.rtv
Rietveld powder data: contains datablock V. DOI: 10.1107/S0108768112039961/dk5006Vsup6.rtv
Program(s) used to refine structure: Jana2000 (Petricek, Dusek & Palatinus, 2000) for (IV), (V). Software used to prepare material for publication: Jana2000 (Petricek, Dusek & Palatinus, 2000) for (IV), (V).
Ag_{0.034}In_{0.037}Sb_{0.764}Te_{0.165}  Z = 3 
M_{r} = 122  F(000) = 1834 
Trigonal, R3m(00γ)00†  D_{x} = 6.709 Mg m^{−}^{3} 
q = 1.500000c*  ? radiation, λ = 0.41873 Å 
a = 4.3037 (5) Å  T = 545 K 
c = 5.6452 (6) Å  ?, ? × ? × ? mm 
V = 90.55 (2) Å^{3} 
† Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (4) x_{2}, x_{1}, −x_{3}, −x_{4}; (5) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (6) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (10) −x_{2}, −x_{1}, x_{3}, x_{4}; (11) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (12) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (13) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (14) −x_{2}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (15) −x_{1}+x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (16) x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (17) x_{1}−x_{2}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (18) −x_{1}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (19) −x_{1}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (20) x_{2}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (21) x_{1}−x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (22) −x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (23) −x_{1}+x_{2}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (24) x_{1}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (25) x_{1}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (26) −x_{2}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}; (27) −x_{1}+x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (28) x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (29) x_{1}−x_{2}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (30) −x_{1}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (31) −x_{1}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (32) x_{2}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (33) x_{1}−x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (34) −x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (35) −x_{1}+x_{2}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (36) x_{1}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}. 
R_{p} = 0.020  56 parameters 
R_{wp} = 0.029  0 restraints 
R_{exp} = 0.030  12 constraints 
R(F) = 0.013  Weighting scheme based on measured s.u.'s 
χ^{2} = 0.960  (Δ/σ)_{max} = 7.061 
2601 data points  Background function: 36 Legendre polynoms 
Profile function: PseudoVoigt  Preferred orientation correction: none 
Ag_{0.034}In_{0.037}Sb_{0.764}Te_{0.165}  V = 90.55 (2) Å^{3} 
M_{r} = 122  Z = 3 
Trigonal, R3m(00γ)00†  ? radiation, λ = 0.41873 Å 
q = 1.500000c*  T = 545 K 
a = 4.3037 (5) Å  ?, ? × ? × ? mm 
c = 5.6452 (6) Å 
† Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (4) x_{2}, x_{1}, −x_{3}, −x_{4}; (5) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (6) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (10) −x_{2}, −x_{1}, x_{3}, x_{4}; (11) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (12) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (13) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (14) −x_{2}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (15) −x_{1}+x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (16) x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (17) x_{1}−x_{2}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (18) −x_{1}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (19) −x_{1}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (20) x_{2}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (21) x_{1}−x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (22) −x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (23) −x_{1}+x_{2}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (24) x_{1}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (25) x_{1}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (26) −x_{2}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}; (27) −x_{1}+x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (28) x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (29) x_{1}−x_{2}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (30) −x_{1}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (31) −x_{1}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (32) x_{2}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (33) x_{1}−x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (34) −x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (35) −x_{1}+x_{2}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (36) x_{1}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}. 
R_{p} = 0.020  2601 data points 
R_{wp} = 0.029  56 parameters 
R_{exp} = 0.030  0 restraints 
R(F) = 0.013  (Δ/σ)_{max} = 7.061 
χ^{2} = 0.960 
x  y  z  U_{iso}*/U_{eq}  Occ. (<1)  
Sb1  0  0  0  0.0296 (6)  0.764 
Te1  0  0  0  0.0296 (5)  0.165 
Ag1  0  0  0  0.0296 (5)  0.034 
In1  0  0  0  0.0296 (5)  0.037 
U^{11}  U^{22}  U^{33}  U^{12}  U^{13}  U^{23}  
Sb1  0.0229 (5)  0.0229 (5)  0.0431 (14)  0.0114 (2)  0  0 
Te1  0.0229 (5)  0.022892  0.0431 (14)  0.011446  0  0 
Ag1  0.0229 (5)  0.022892  0.0431 (14)  0.011446  0  0 
In1  0.0229 (5)  0.022892  0.0431 (14)  0.011446  0  0 
Sb_{0.89}Te_{0.11}  Z = 3 
M_{r} = 122.4  F(000) = 800 
Trigonal, R3m(00γ)00†  D_{x} = 6.716 Mg m^{−}^{3} 
q = 1.551587c*  ? radiation, λ = 0.41873 Å 
a = 4.29686 (13) Å  T = 293 K 
c = 5.67590 (19) Å  ?, ? × ? × ? mm 
V = 90.75 (1) Å^{3} 
† Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (4) x_{2}, x_{1}, −x_{3}, −x_{4}; (5) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (6) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (10) −x_{2}, −x_{1}, x_{3}, x_{4}; (11) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (12) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (13) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (14) −x_{2}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (15) −x_{1}+x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (16) x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (17) x_{1}−x_{2}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (18) −x_{1}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (19) −x_{1}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (20) x_{2}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (21) x_{1}−x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (22) −x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (23) −x_{1}+x_{2}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (24) x_{1}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (25) x_{1}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (26) −x_{2}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}; (27) −x_{1}+x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (28) x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (29) x_{1}−x_{2}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (30) −x_{1}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (31) −x_{1}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (32) x_{2}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (33) x_{1}−x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (34) −x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (35) −x_{1}+x_{2}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (36) x_{1}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}. 
R_{p} = 0.021  68 parameters 
R_{wp} = 0.030  0 restraints 
R_{exp} = 0.030  4 constraints 
R(F) = 0.016  Weighting scheme based on measured s.u.'s 
χ^{2} = 1.000  (Δ/σ)_{max} = 5.113 
3661 data points  Background function: 36 Legendre polynoms 
Profile function: PseudoVoigt  Preferred orientation correction: March & Dollase 
Sb_{0.89}Te_{0.11}  V = 90.75 (1) Å^{3} 
M_{r} = 122.4  Z = 3 
Trigonal, R3m(00γ)00†  ? radiation, λ = 0.41873 Å 
q = 1.551587c*  T = 293 K 
a = 4.29686 (13) Å  ?, ? × ? × ? mm 
c = 5.67590 (19) Å 
† Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (4) x_{2}, x_{1}, −x_{3}, −x_{4}; (5) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (6) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (10) −x_{2}, −x_{1}, x_{3}, x_{4}; (11) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (12) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (13) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (14) −x_{2}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (15) −x_{1}+x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (16) x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (17) x_{1}−x_{2}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (18) −x_{1}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (19) −x_{1}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (20) x_{2}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (21) x_{1}−x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (22) −x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (23) −x_{1}+x_{2}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (24) x_{1}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (25) x_{1}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (26) −x_{2}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}; (27) −x_{1}+x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (28) x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (29) x_{1}−x_{2}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (30) −x_{1}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (31) −x_{1}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (32) x_{2}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (33) x_{1}−x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (34) −x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (35) −x_{1}+x_{2}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (36) x_{1}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}. 
R_{p} = 0.021  3661 data points 
R_{wp} = 0.030  68 parameters 
R_{exp} = 0.030  0 restraints 
R(F) = 0.016  (Δ/σ)_{max} = 5.113 
χ^{2} = 1.000 
x  y  z  U_{iso}*/U_{eq}  Occ. (<1)  
Sb1  0  0  0  0.0116 (3)  0.887 
Te1  0  0  0  0.0116 (3)  0.113 
U^{11}  U^{22}  U^{33}  U^{12}  U^{13}  U^{23}  
Sb1  0.0123 (2)  0.0123 (2)  0.0101 (7)  0.00614 (12)  0  0 
Te1  0.0123 (2)  0.012285  0.0101 (7)  0.006143  0  0 
AgInTe_{2}  Z = 4 
M_{r} = 477.9  F(000) = 800 
Tetragonal, I42d  D_{x} = 6.092 Mg m^{−}^{3} 
Hall symbol: I 4;2bw  ? radiation, λ = 0.41873 Å 
a = 6.4275 (3) Å  T = 293 K 
c = 12.6089 (9) Å  ?, ? × ? × ? mm 
V = 520.91 (5) Å^{3} 
R_{p} = 0.021  68 parameters 
R_{wp} = 0.030  0 restraints 
R_{exp} = 0.030  4 constraints 
R(F) = 0.016  Weighting scheme based on measured s.u.'s 
χ^{2} = 1.000  (Δ/σ)_{max} = 5.113 
3661 data points  Background function: 36 Legendre polynoms 
Profile function: PseudoVoigt  Preferred orientation correction: none 
AgInTe_{2}  V = 520.91 (5) Å^{3} 
M_{r} = 477.9  Z = 4 
Tetragonal, I42d  ? radiation, λ = 0.41873 Å 
a = 6.4275 (3) Å  T = 293 K 
c = 12.6089 (9) Å  ?, ? × ? × ? mm 
R_{p} = 0.021  3661 data points 
R_{wp} = 0.030  68 parameters 
R_{exp} = 0.030  0 restraints 
R(F) = 0.016  (Δ/σ)_{max} = 5.113 
χ^{2} = 1.000 
x  y  z  U_{iso}*/U_{eq}  
Ag1  0  0  0.5  0.0289 (13)*  
In1  0  0  0  0.0289 (13)*  
Te2  0.252 (11)  0.25  0.125  0.0289 (13)* 
Sb_{0.87}Te_{0.13}  Z = 3 
M_{r} = 122.5  F(000) = 1841 
Trigonal, R3m(00γ)00†  D_{x} = 6.598 Mg m^{−}^{3} 
q = 1.56522c*  Xray radiation, λ = 0.41853 Å 
a = 4.3181 Å  T = 773 K 
c = 5.7267 Å  ?, ? × ? × ? mm 
V = 92.47 Å^{3} 
† Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{2}, −x_{1}, x_{3}, x_{4}; (4) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (5) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (6) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{2}, x_{1}, −x_{3}, −x_{4}; (10) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (11) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (12) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (13) 2/3+x_{1}, 1/3+x_{2}, 1/3+x_{3}, x_{4}; (14) 2/3−x_{2}, 1/3+x_{1}−x_{2}, 1/3+x_{3}, x_{4}; (15) 2/3−x_{2}, 1/3−x_{1}, 1/3+x_{3}, x_{4}; (16) 2/3−x_{1}+x_{2}, 1/3−x_{1}, 1/3+x_{3}, x_{4}; (17) 2/3+x_{1}, 1/3+x_{1}−x_{2}, 1/3+x_{3}, x_{4}; (18) 2/3−x_{1}+x_{2}, 1/3+x_{2}, 1/3+x_{3}, x_{4}; (19) 2/3−x_{1}, 1/3−x_{2}, 1/3−x_{3}, −x_{4}; (20) 2/3+x_{2}, 1/3−x_{1}+x_{2}, 1/3−x_{3}, −x_{4}; (21) 2/3+x_{2}, 1/3+x_{1}, 1/3−x_{3}, −x_{4}; (22) 2/3+x_{1}−x_{2}, 1/3+x_{1}, 1/3−x_{3}, −x_{4}; (23) 2/3−x_{1}, 1/3−x_{1}+x_{2}, 1/3−x_{3}, −x_{4}; (24) 2/3+x_{1}−x_{2}, 1/3−x_{2}, 1/3−x_{3}, −x_{4}; (25) 1/3+x_{1}, 2/3+x_{2}, 2/3+x_{3}, x_{4}; (26) 1/3−x_{2}, 2/3+x_{1}−x_{2}, 2/3+x_{3}, x_{4}; (27) 1/3−x_{2}, 2/3−x_{1}, 2/3+x_{3}, x_{4}; (28) 1/3−x_{1}+x_{2}, 2/3−x_{1}, 2/3+x_{3}, x_{4}; (29) 1/3+x_{1}, 2/3+x_{1}−x_{2}, 2/3+x_{3}, x_{4}; (30) 1/3−x_{1}+x_{2}, 2/3+x_{2}, 2/3+x_{3}, x_{4}; (31) 1/3−x_{1}, 2/3−x_{2}, 2/3−x_{3}, −x_{4}; (32) 1/3+x_{2}, 2/3−x_{1}+x_{2}, 2/3−x_{3}, −x_{4}; (33) 1/3+x_{2}, 2/3+x_{1}, 2/3−x_{3}, −x_{4}; (34) 1/3+x_{1}−x_{2}, 2/3+x_{1}, 2/3−x_{3}, −x_{4}; (35) 1/3−x_{1}, 2/3−x_{1}+x_{2}, 2/3−x_{3}, −x_{4}; (36) 1/3+x_{1}−x_{2}, 2/3−x_{2}, 2/3−x_{3}, −x_{4}. 
R_{p} = 0.020  Profile function: PseudoVoigt 
R_{wp} = 0.029  59 parameters 
R_{exp} = 0.024  Weighting scheme based on measured s.u.'s 
R(F) = 0.030  (Δ/σ)_{max} = 0.628 
χ^{2} = NOT FOUND  Background function: 36 Legendre polynoms 
1375 data points  Preferred orientation correction: none 
Sb_{0.87}Te_{0.13}  V = 92.47 Å^{3} 
M_{r} = 122.5  Z = 3 
Trigonal, R3m(00γ)00†  Xray radiation, λ = 0.41853 Å 
q = 1.56522c*  T = 773 K 
a = 4.3181 Å  ?, ? × ? × ? mm 
c = 5.7267 Å 
† Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{2}, −x_{1}, x_{3}, x_{4}; (4) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (5) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (6) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{2}, x_{1}, −x_{3}, −x_{4}; (10) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (11) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (12) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (13) 2/3+x_{1}, 1/3+x_{2}, 1/3+x_{3}, x_{4}; (14) 2/3−x_{2}, 1/3+x_{1}−x_{2}, 1/3+x_{3}, x_{4}; (15) 2/3−x_{2}, 1/3−x_{1}, 1/3+x_{3}, x_{4}; (16) 2/3−x_{1}+x_{2}, 1/3−x_{1}, 1/3+x_{3}, x_{4}; (17) 2/3+x_{1}, 1/3+x_{1}−x_{2}, 1/3+x_{3}, x_{4}; (18) 2/3−x_{1}+x_{2}, 1/3+x_{2}, 1/3+x_{3}, x_{4}; (19) 2/3−x_{1}, 1/3−x_{2}, 1/3−x_{3}, −x_{4}; (20) 2/3+x_{2}, 1/3−x_{1}+x_{2}, 1/3−x_{3}, −x_{4}; (21) 2/3+x_{2}, 1/3+x_{1}, 1/3−x_{3}, −x_{4}; (22) 2/3+x_{1}−x_{2}, 1/3+x_{1}, 1/3−x_{3}, −x_{4}; (23) 2/3−x_{1}, 1/3−x_{1}+x_{2}, 1/3−x_{3}, −x_{4}; (24) 2/3+x_{1}−x_{2}, 1/3−x_{2}, 1/3−x_{3}, −x_{4}; (25) 1/3+x_{1}, 2/3+x_{2}, 2/3+x_{3}, x_{4}; (26) 1/3−x_{2}, 2/3+x_{1}−x_{2}, 2/3+x_{3}, x_{4}; (27) 1/3−x_{2}, 2/3−x_{1}, 2/3+x_{3}, x_{4}; (28) 1/3−x_{1}+x_{2}, 2/3−x_{1}, 2/3+x_{3}, x_{4}; (29) 1/3+x_{1}, 2/3+x_{1}−x_{2}, 2/3+x_{3}, x_{4}; (30) 1/3−x_{1}+x_{2}, 2/3+x_{2}, 2/3+x_{3}, x_{4}; (31) 1/3−x_{1}, 2/3−x_{2}, 2/3−x_{3}, −x_{4}; (32) 1/3+x_{2}, 2/3−x_{1}+x_{2}, 2/3−x_{3}, −x_{4}; (33) 1/3+x_{2}, 2/3+x_{1}, 2/3−x_{3}, −x_{4}; (34) 1/3+x_{1}−x_{2}, 2/3+x_{1}, 2/3−x_{3}, −x_{4}; (35) 1/3−x_{1}, 2/3−x_{1}+x_{2}, 2/3−x_{3}, −x_{4}; (36) 1/3+x_{1}−x_{2}, 2/3−x_{2}, 2/3−x_{3}, −x_{4}. 
R_{p} = 0.020  χ^{2} = NOT FOUND 
R_{wp} = 0.029  1375 data points 
R_{exp} = 0.024  59 parameters 
R(F) = 0.030  (Δ/σ)_{max} = 0.628 
x  y  z  U_{iso}*/U_{eq}  Occ. (<1)  
Sb1  0  0  0  0.03832 (14)  0.870 
Te1  0  0  0  0.03832 (12)  0.130 
U^{11}  U^{22}  U^{33}  U^{12}  U^{13}  U^{23}  
Sb1  0.03681 (14)  0.03681 (14)  0.0413 (3)  0.01841 (7)  0  0 
Te1  0.03681 (14)  0.03681  0.0413 (3)  0.018405  0  0 
Average  Minimum  Maximum  
Sb1—Sb1^{i}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{ii}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{iii}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{iv}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{v}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{vi}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Te1^{i}  3.1483 (6)  2.8798 (9)  3.4307 (9) 
Sb1—Te1^{ii}  3.1483 (6)  2.8798 (9)  3.4307 (9) 
Sb1—Te1^{iii}  3.1483 (6)  2.8798 (9)  3.4307 (9) 
Sb1—Te1^{iv}  3.1491 (6)  2.8804 (9)  3.4316 (9) 
Sb1—Te1^{v}  3.1491 (6)  2.8804 (9)  3.4316 (9) 
Sb1—Te1^{vi}  3.1491 (6)  2.8804 (9)  3.4316 (9) 
Symmetry codes: (i) x_{1}−1/3, x_{2}−2/3, x_{3}+1/3, x_{4}; (ii) x_{1}−1/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (iii) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (iv) x_{1}−2/3, x_{2}−1/3, x_{3}−1/3, x_{4}; (v) x_{1}+1/3, x_{2}−1/3, x_{3}−1/3, x_{4}; (vi) x_{1}+1/3, x_{2}+2/3, x_{3}−1/3, x_{4}. 
Sb_{2}O_{3}  Z = 16 
M_{r} = 291.5  F(000) = 1841 
Cubic, Fd3m  D_{x} = 5.442 Mg m^{−}^{3} 
Hall symbol: F 4vw;2vw;3  Xray radiation, λ = 0.41853 Å 
a = 11.2471 Å  T = 773 K 
V = 1422.71 Å^{3}  ?, ? × ? × ? mm 
R_{p} = 0.020  Profile function: PseudoVoigt 
R_{wp} = 0.029  59 parameters 
R_{exp} = 0.024  Weighting scheme based on measured s.u.'s 
R(F) = 0.030  (Δ/σ)_{max} = 0.628 
χ^{2} = NOT FOUND  Background function: 36 Legendre polynoms 
1375 data points  Preferred orientation correction: none 
Sb_{2}O_{3}  Z = 16 
M_{r} = 291.5  Xray radiation, λ = 0.41853 Å 
Cubic, Fd3m  T = 773 K 
a = 11.2471 Å  ?, ? × ? × ? mm 
V = 1422.71 Å^{3} 
R_{p} = 0.020  χ^{2} = NOT FOUND 
R_{wp} = 0.029  1375 data points 
R_{exp} = 0.024  59 parameters 
R(F) = 0.030  (Δ/σ)_{max} = 0.628 
x  y  z  U_{iso}*/U_{eq}  
Sb2  0.88704 (13)  0.88704 (13)  0.88704 (13)  0.0264 (14)*  
O1  0.188 (2)  0  0  0.0264 (14)* 
Sb2—O1^{i}  1.986 (10)  O1—O1^{viii}  2.99 (2) 
Sb2—O1^{ii}  2.936 (16)  O1—O1^{ix}  2.979 (8) 
Sb2—O1^{iii}  2.936 (16)  O1—O1^{x}  2.99 (2) 
Sb2—O1^{iv}  1.986 (10)  O1—O1^{xi}  2.979 (8) 
Sb2—O1^{v}  2.936 (16)  O1—O1^{xii}  2.99 (2) 
Sb2—O1^{vi}  1.986 (10)  O1—O1^{xiii}  2.979 (8) 
O1—O1^{vii}  2.979 (8)  O1—O1^{xiv}  2.99 (2) 
Symmetry codes: (i) −x+1, −y+1, z+1; (ii) −x+5/4, z+3/4, y+3/4; (iii) y+3/4, −x+5/4, z+3/4; (iv) −z+1, −x+1, y+1; (v) z+3/4, y+3/4, −x+5/4; (vi) −y+1, z+1, −x+1; (vii) −y+1/4, x−1/4, z−1/4; (viii) z, x, y; (ix) y+1/4, −x+1/4, z+1/4; (x) −z, −x, y; (xi) z+1/4, −y−1/4, x−1/4; (xii) y, z, x; (xiii) z+1/4, y+1/4, −x+1/4; (xiv) −y, z, −x. 
Experimental details
(I)  (II)  (III)  (IV)  
Crystal data  
Chemical formula  Ag_{0.034}In_{0.037}Sb_{0.764}Te_{0.165}  Sb_{0.89}Te_{0.11}  AgInTe_{2}  Sb_{0.87}Te_{0.13} 
M_{r}  122  122.4  477.9  122.5 
Crystal system, space group  Trigonal, R3m(00γ)00†  Trigonal, R3m(00γ)00‡  Tetragonal, I42d  Trigonal, R3m(00γ)00§ 
Temperature (K)  545  293  293  773 
Wave vectors  q = 1.500000c*  q = 1.551587c*  I 4;2bw  q = 1.56522c* 
a, b, c (Å)  4.3037 (5), 4.3037 (5), 5.6452 (6)  4.29686 (13), 4.29686 (13), 5.67590 (19)  90, 90, 90  4.3181, 4.3181, 5.7267 
α, β, γ (°)  90, 90, 120  90, 90, 120  520.91 (5)  90, 90, 120 
V (Å^{3})  90.55 (2)  90.75 (1)  4  92.47 
Z  3  3  800  3 
Radiation type  ?, λ = 0.41873 Å  ?, λ = 0.41873 Å  –  Xray, λ = 0.41853 Å 
µ (mm^{−}^{1})  –  –  ?  – 
Specimen shape, size (mm)  ?, ? × ? × ?  ?, ? × ? × ?  ?, ? × ? × ?  
Data collection  
Diffractometer  ?  ?  ?  ? 
Specimen mounting  ?  ?  ?  ? 
Data collection mode  ?  ?  ?  ? 
Scan method  ?  ?  ?  ? 
2θ values (°)  2θ_{min} = 5.5 2θ_{max} = 31.5 2θ_{step} = 0.01  2θ_{min} = 5.5 2θ_{max} = 42.1 2θ_{step} = 0.01  2θ_{min} = 5.5 2θ_{max} = 42.1 2θ_{step} = 0.01  2θ_{min} = 3.02 2θ_{max} = 30.5 2θ_{step} = 0.02 
Refinement  
R factors and goodness of fit  R_{p} = 0.020, R_{wp} = 0.029, R_{exp} = 0.030, R(F) = 0.013, χ^{2} = 0.960  R_{p} = 0.021, R_{wp} = 0.030, R_{exp} = 0.030, R(F) = 0.016, χ^{2} = 1.000  R_{p} = 0.021, R_{wp} = 0.030, R_{exp} = 0.030, R(F) = 0.016, χ^{2} = 1.000  R_{p} = 0.020, R_{wp} = 0.029, R_{exp} = 0.024, R(F) = 0.030, χ^{2} = NOT FOUND 
No. of data points  2601  3661  3661  1375 
No. of parameters  56  68  68  59 
No. of restraints  0  0  0  ? 
(Δ/σ)_{max}  7.061  5.113  5.113  0.628 
(V)  
Crystal data  
Chemical formula  Sb_{2}O_{3} 
M_{r}  291.5 
Crystal system, space group  Cubic, Fd3m 
Temperature (K)  773 
Wave vectors  F 4vw;2vw;3 
a, b, c (Å)  90, 90, 90 
α, β, γ (°)  1422.71 
V (Å^{3})  16 
Z  1841 
Radiation type  – 
µ (mm^{−}^{1})  ? 
Specimen shape, size (mm)  
Data collection  
Diffractometer  ? 
Specimen mounting  ? 
Data collection mode  ? 
Scan method  ? 
2θ values (°)  2θ_{min} = 3.02 2θ_{max} = 30.5 2θ_{step} = 0.02 
Refinement  
R factors and goodness of fit  R_{p} = 0.020, R_{wp} = 0.029, R_{exp} = 0.024, R(F) = 0.030, χ^{2} = NOT FOUND 
No. of data points  1375 
No. of parameters  59 
No. of restraints  ? 
(Δ/σ)_{max}  0.628 
† Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (4) x_{2}, x_{1}, −x_{3}, −x_{4}; (5) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (6) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (10) −x_{2}, −x_{1}, x_{3}, x_{4}; (11) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (12) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (13) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (14) −x_{2}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (15) −x_{1}+x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (16) x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (17) x_{1}−x_{2}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (18) −x_{1}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (19) −x_{1}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (20) x_{2}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (21) x_{1}−x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (22) −x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (23) −x_{1}+x_{2}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (24) x_{1}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (25) x_{1}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (26) −x_{2}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}; (27) −x_{1}+x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (28) x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (29) x_{1}−x_{2}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (30) −x_{1}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (31) −x_{1}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (32) x_{2}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (33) x_{1}−x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (34) −x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (35) −x_{1}+x_{2}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (36) x_{1}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}.
‡ Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (4) x_{2}, x_{1}, −x_{3}, −x_{4}; (5) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (6) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (10) −x_{2}, −x_{1}, x_{3}, x_{4}; (11) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (12) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (13) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (14) −x_{2}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (15) −x_{1}+x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (16) x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (17) x_{1}−x_{2}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (18) −x_{1}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (19) −x_{1}+2/3, −x_{2}+1/3, −x_{3}+1/3, −x_{4}; (20) x_{2}+2/3, −x_{1}+x_{2}+1/3, −x_{3}+1/3, −x_{4}; (21) x_{1}−x_{2}+2/3, x_{1}+1/3, −x_{3}+1/3, −x_{4}; (22) −x_{2}+2/3, −x_{1}+1/3, x_{3}+1/3, x_{4}; (23) −x_{1}+x_{2}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (24) x_{1}+2/3, x_{1}−x_{2}+1/3, x_{3}+1/3, x_{4}; (25) x_{1}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (26) −x_{2}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}; (27) −x_{1}+x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (28) x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (29) x_{1}−x_{2}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (30) −x_{1}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (31) −x_{1}+1/3, −x_{2}+2/3, −x_{3}+2/3, −x_{4}; (32) x_{2}+1/3, −x_{1}+x_{2}+2/3, −x_{3}+2/3, −x_{4}; (33) x_{1}−x_{2}+1/3, x_{1}+2/3, −x_{3}+2/3, −x_{4}; (34) −x_{2}+1/3, −x_{1}+2/3, x_{3}+2/3, x_{4}; (35) −x_{1}+x_{2}+1/3, x_{2}+2/3, x_{3}+2/3, x_{4}; (36) x_{1}+1/3, x_{1}−x_{2}+2/3, x_{3}+2/3, x_{4}.
§ Symmetry operations: (1) x_{1}, x_{2}, x_{3}, x_{4}; (2) −x_{2}, x_{1}−x_{2}, x_{3}, x_{4}; (3) −x_{2}, −x_{1}, x_{3}, x_{4}; (4) −x_{1}+x_{2}, −x_{1}, x_{3}, x_{4}; (5) x_{1}, x_{1}−x_{2}, x_{3}, x_{4}; (6) −x_{1}+x_{2}, x_{2}, x_{3}, x_{4}; (7) −x_{1}, −x_{2}, −x_{3}, −x_{4}; (8) x_{2}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (9) x_{2}, x_{1}, −x_{3}, −x_{4}; (10) x_{1}−x_{2}, x_{1}, −x_{3}, −x_{4}; (11) −x_{1}, −x_{1}+x_{2}, −x_{3}, −x_{4}; (12) x_{1}−x_{2}, −x_{2}, −x_{3}, −x_{4}; (13) 2/3+x_{1}, 1/3+x_{2}, 1/3+x_{3}, x_{4}; (14) 2/3−x_{2}, 1/3+x_{1}−x_{2}, 1/3+x_{3}, x_{4}; (15) 2/3−x_{2}, 1/3−x_{1}, 1/3+x_{3}, x_{4}; (16) 2/3−x_{1}+x_{2}, 1/3−x_{1}, 1/3+x_{3}, x_{4}; (17) 2/3+x_{1}, 1/3+x_{1}−x_{2}, 1/3+x_{3}, x_{4}; (18) 2/3−x_{1}+x_{2}, 1/3+x_{2}, 1/3+x_{3}, x_{4}; (19) 2/3−x_{1}, 1/3−x_{2}, 1/3−x_{3}, −x_{4}; (20) 2/3+x_{2}, 1/3−x_{1}+x_{2}, 1/3−x_{3}, −x_{4}; (21) 2/3+x_{2}, 1/3+x_{1}, 1/3−x_{3}, −x_{4}; (22) 2/3+x_{1}−x_{2}, 1/3+x_{1}, 1/3−x_{3}, −x_{4}; (23) 2/3−x_{1}, 1/3−x_{1}+x_{2}, 1/3−x_{3}, −x_{4}; (24) 2/3+x_{1}−x_{2}, 1/3−x_{2}, 1/3−x_{3}, −x_{4}; (25) 1/3+x_{1}, 2/3+x_{2}, 2/3+x_{3}, x_{4}; (26) 1/3−x_{2}, 2/3+x_{1}−x_{2}, 2/3+x_{3}, x_{4}; (27) 1/3−x_{2}, 2/3−x_{1}, 2/3+x_{3}, x_{4}; (28) 1/3−x_{1}+x_{2}, 2/3−x_{1}, 2/3+x_{3}, x_{4}; (29) 1/3+x_{1}, 2/3+x_{1}−x_{2}, 2/3+x_{3}, x_{4}; (30) 1/3−x_{1}+x_{2}, 2/3+x_{2}, 2/3+x_{3}, x_{4}; (31) 1/3−x_{1}, 2/3−x_{2}, 2/3−x_{3}, −x_{4}; (32) 1/3+x_{2}, 2/3−x_{1}+x_{2}, 2/3−x_{3}, −x_{4}; (33) 1/3+x_{2}, 2/3+x_{1}, 2/3−x_{3}, −x_{4}; (34) 1/3+x_{1}−x_{2}, 2/3+x_{1}, 2/3−x_{3}, −x_{4}; (35) 1/3−x_{1}, 2/3−x_{1}+x_{2}, 2/3−x_{3}, −x_{4}; (36) 1/3+x_{1}−x_{2}, 2/3−x_{2}, 2/3−x_{3}, −x_{4}.
Computer programs: Jana2000 (Petricek, Dusek & Palatinus, 2000).
Average  Minimum  Maximum  
Sb1—Sb1^{i}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{ii}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{iii}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{iv}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{v}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Sb1^{vi}  3.1499 (14)  2.9339 (7)  3.3530 (8) 
Sb1—Te1^{i}  3.1483 (6)  2.8798 (9)  3.4307 (9) 
Sb1—Te1^{ii}  3.1483 (6)  2.8798 (9)  3.4307 (9) 
Sb1—Te1^{iii}  3.1483 (6)  2.8798 (9)  3.4307 (9) 
Sb1—Te1^{iv}  3.1491 (6)  2.8804 (9)  3.4316 (9) 
Sb1—Te1^{v}  3.1491 (6)  2.8804 (9)  3.4316 (9) 
Sb1—Te1^{vi}  3.1491 (6)  2.8804 (9)  3.4316 (9) 
Symmetry codes: (i) x_{1}−1/3, x_{2}−2/3, x_{3}+1/3, x_{4}; (ii) x_{1}−1/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (iii) x_{1}+2/3, x_{2}+1/3, x_{3}+1/3, x_{4}; (iv) x_{1}−2/3, x_{2}−1/3, x_{3}−1/3, x_{4}; (v) x_{1}+1/3, x_{2}−1/3, x_{3}−1/3, x_{4}; (vi) x_{1}+1/3, x_{2}+2/3, x_{3}−1/3, x_{4}. 
Sb2—O1^{i}  1.986 (10)  O1—O1^{viii}  2.99 (2) 
Sb2—O1^{ii}  2.936 (16)  O1—O1^{ix}  2.979 (8) 
Sb2—O1^{iii}  2.936 (16)  O1—O1^{x}  2.99 (2) 
Sb2—O1^{iv}  1.986 (10)  O1—O1^{xi}  2.979 (8) 
Sb2—O1^{v}  2.936 (16)  O1—O1^{xii}  2.99 (2) 
Sb2—O1^{vi}  1.986 (10)  O1—O1^{xiii}  2.979 (8) 
O1—O1^{vii}  2.979 (8)  O1—O1^{xiv}  2.99 (2) 
Symmetry codes: (i) −x+1, −y+1, z+1; (ii) −x+5/4, z+3/4, y+3/4; (iii) y+3/4, −x+5/4, z+3/4; (iv) −z+1, −x+1, y+1; (v) z+3/4, y+3/4, −x+5/4; (vi) −y+1, z+1, −x+1; (vii) −y+1/4, x−1/4, z−1/4; (viii) z, x, y; (ix) y+1/4, −x+1/4, z+1/4; (x) −z, −x, y; (xi) z+1/4, −y−1/4, x−1/4; (xii) y, z, x; (xiii) z+1/4, y+1/4, −x+1/4; (xiv) −y, z, −x. 
Acknowledgements
The synchrotron radiation experiments were performed on BL02B2 at SPring8 with the approval of the Japan Synchrotron Radiation Research Institute (proposal Nos. 2010B0084, 2010B1827 and 2011B0030. We express our sincere gratitude to Dr J. Kim at JASRI and to graduate students K. Shakudo, Y. Sato and T. Tachizawa of the Graduate School of Science at Osaka Prefecture University for their assistance with the experiments. The structural models in Fig. 7 were displayed using the Java Structure Viewer (JSV 1.08 lite) created by Dr Steffen Weber.
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