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The crystal structure of a phase-change recording material (the compound Ag3.4In3.7Sb76.4Te16.5) 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 SPring-8. The amorphous phase of this material turns into a crystalline phase at around 416 K; this crystalline phase has an A7-type structure with atoms of Ag, In, Sb or Te randomly occupying the 6c site in the space group. This structure was maintained up to around 545 K as a single phase, although thermal expansion of the crystal lattice was observed. However, above this temperature, phase separation into AgInTe2 and Sb–Te transpired. The first fragment, AgInTe2, reliably maintained its crystal structure 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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112039961/dk5006sup1.cif
Contains datablocks global, I, II, III, IV, V

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768112039961/dk5006Isup2.rtv
Contains datablock I

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768112039961/dk5006IIsup3.rtv
Contains datablock II

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768112039961/dk5006IIIsup4.rtv
Contains datablock III

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768112039961/dk5006IVsup5.rtv
Contains datablock IV

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768112039961/dk5006Vsup6.rtv
Contains datablock V

B-IncStrDB reference: 6732EXfQbW

Computing details top

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
(I) top
Crystal data top
Ag0.034In0.037Sb0.764Te0.165Z = 3
Mr = 122F(000) = 1834
Trigonal, R3m(00γ)00†Dx = 6.709 Mg m3
q = 1.500000c*? radiation, λ = 0.41873 Å
a = 4.3037 (5) ÅT = 545 K
c = 5.6452 (6) Å?, ? × ? × ? mm
V = 90.55 (2) Å3
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x1+x2, −x1, x3, x4; (4) x2, x1, −x3, −x4; (5) x1x2, −x2, −x3, −x4; (6) −x1, −x1+x2, −x3, −x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x1x2, x1, −x3, −x4; (10) −x2, −x1, x3, x4; (11) −x1+x2, x2, x3, x4; (12) x1, x1x2, x3, x4; (13) x1+2/3, x2+1/3, x3+1/3, x4; (14) −x2+2/3, x1x2+1/3, x3+1/3, x4; (15) −x1+x2+2/3, −x1+1/3, x3+1/3, x4; (16) x2+2/3, x1+1/3, −x3+1/3, −x4; (17) x1x2+2/3, −x2+1/3, −x3+1/3, −x4; (18) −x1+2/3, −x1+x2+1/3, −x3+1/3, −x4; (19) −x1+2/3, −x2+1/3, −x3+1/3, −x4; (20) x2+2/3, −x1+x2+1/3, −x3+1/3, −x4; (21) x1x2+2/3, x1+1/3, −x3+1/3, −x4; (22) −x2+2/3, −x1+1/3, x3+1/3, x4; (23) −x1+x2+2/3, x2+1/3, x3+1/3, x4; (24) x1+2/3, x1x2+1/3, x3+1/3, x4; (25) x1+1/3, x2+2/3, x3+2/3, x4; (26) −x2+1/3, x1x2+2/3, x3+2/3, x4; (27) −x1+x2+1/3, −x1+2/3, x3+2/3, x4; (28) x2+1/3, x1+2/3, −x3+2/3, −x4; (29) x1x2+1/3, −x2+2/3, −x3+2/3, −x4; (30) −x1+1/3, −x1+x2+2/3, −x3+2/3, −x4; (31) −x1+1/3, −x2+2/3, −x3+2/3, −x4; (32) x2+1/3, −x1+x2+2/3, −x3+2/3, −x4; (33) x1x2+1/3, x1+2/3, −x3+2/3, −x4; (34) −x2+1/3, −x1+2/3, x3+2/3, x4; (35) −x1+x2+1/3, x2+2/3, x3+2/3, x4; (36) x1+1/3, x1x2+2/3, x3+2/3, x4.

Data collection top
2θmin = 5.5°, 2θmax = 31.5°, 2θstep = 0.01°
Refinement top
Rp = 0.02056 parameters
Rwp = 0.0290 restraints
Rexp = 0.03012 constraints
R(F) = 0.013Weighting scheme based on measured s.u.'s
χ2 = 0.960(Δ/σ)max = 7.061
2601 data pointsBackground function: 36 Legendre polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Crystal data top
Ag0.034In0.037Sb0.764Te0.165V = 90.55 (2) Å3
Mr = 122Z = 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) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x1+x2, −x1, x3, x4; (4) x2, x1, −x3, −x4; (5) x1x2, −x2, −x3, −x4; (6) −x1, −x1+x2, −x3, −x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x1x2, x1, −x3, −x4; (10) −x2, −x1, x3, x4; (11) −x1+x2, x2, x3, x4; (12) x1, x1x2, x3, x4; (13) x1+2/3, x2+1/3, x3+1/3, x4; (14) −x2+2/3, x1x2+1/3, x3+1/3, x4; (15) −x1+x2+2/3, −x1+1/3, x3+1/3, x4; (16) x2+2/3, x1+1/3, −x3+1/3, −x4; (17) x1x2+2/3, −x2+1/3, −x3+1/3, −x4; (18) −x1+2/3, −x1+x2+1/3, −x3+1/3, −x4; (19) −x1+2/3, −x2+1/3, −x3+1/3, −x4; (20) x2+2/3, −x1+x2+1/3, −x3+1/3, −x4; (21) x1x2+2/3, x1+1/3, −x3+1/3, −x4; (22) −x2+2/3, −x1+1/3, x3+1/3, x4; (23) −x1+x2+2/3, x2+1/3, x3+1/3, x4; (24) x1+2/3, x1x2+1/3, x3+1/3, x4; (25) x1+1/3, x2+2/3, x3+2/3, x4; (26) −x2+1/3, x1x2+2/3, x3+2/3, x4; (27) −x1+x2+1/3, −x1+2/3, x3+2/3, x4; (28) x2+1/3, x1+2/3, −x3+2/3, −x4; (29) x1x2+1/3, −x2+2/3, −x3+2/3, −x4; (30) −x1+1/3, −x1+x2+2/3, −x3+2/3, −x4; (31) −x1+1/3, −x2+2/3, −x3+2/3, −x4; (32) x2+1/3, −x1+x2+2/3, −x3+2/3, −x4; (33) x1x2+1/3, x1+2/3, −x3+2/3, −x4; (34) −x2+1/3, −x1+2/3, x3+2/3, x4; (35) −x1+x2+1/3, x2+2/3, x3+2/3, x4; (36) x1+1/3, x1x2+2/3, x3+2/3, x4.

Data collection top
2θmin = 5.5°, 2θmax = 31.5°, 2θstep = 0.01°
Refinement top
Rp = 0.0202601 data points
Rwp = 0.02956 parameters
Rexp = 0.0300 restraints
R(F) = 0.013(Δ/σ)max = 7.061
χ2 = 0.960
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sb10000.0296 (6)0.764
Te10000.0296 (5)0.165
Ag10000.0296 (5)0.034
In10000.0296 (5)0.037
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.0229 (5)0.0229 (5)0.0431 (14)0.0114 (2)00
Te10.0229 (5)0.0228920.0431 (14)0.01144600
Ag10.0229 (5)0.0228920.0431 (14)0.01144600
In10.0229 (5)0.0228920.0431 (14)0.01144600
(II) top
Crystal data top
Sb0.89Te0.11Z = 3
Mr = 122.4F(000) = 800
Trigonal, R3m(00γ)00†Dx = 6.716 Mg m3
q = 1.551587c*? radiation, λ = 0.41873 Å
a = 4.29686 (13) ÅT = 293 K
c = 5.67590 (19) Å?, ? × ? × ? mm
V = 90.75 (1) Å3
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x1+x2, −x1, x3, x4; (4) x2, x1, −x3, −x4; (5) x1x2, −x2, −x3, −x4; (6) −x1, −x1+x2, −x3, −x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x1x2, x1, −x3, −x4; (10) −x2, −x1, x3, x4; (11) −x1+x2, x2, x3, x4; (12) x1, x1x2, x3, x4; (13) x1+2/3, x2+1/3, x3+1/3, x4; (14) −x2+2/3, x1x2+1/3, x3+1/3, x4; (15) −x1+x2+2/3, −x1+1/3, x3+1/3, x4; (16) x2+2/3, x1+1/3, −x3+1/3, −x4; (17) x1x2+2/3, −x2+1/3, −x3+1/3, −x4; (18) −x1+2/3, −x1+x2+1/3, −x3+1/3, −x4; (19) −x1+2/3, −x2+1/3, −x3+1/3, −x4; (20) x2+2/3, −x1+x2+1/3, −x3+1/3, −x4; (21) x1x2+2/3, x1+1/3, −x3+1/3, −x4; (22) −x2+2/3, −x1+1/3, x3+1/3, x4; (23) −x1+x2+2/3, x2+1/3, x3+1/3, x4; (24) x1+2/3, x1x2+1/3, x3+1/3, x4; (25) x1+1/3, x2+2/3, x3+2/3, x4; (26) −x2+1/3, x1x2+2/3, x3+2/3, x4; (27) −x1+x2+1/3, −x1+2/3, x3+2/3, x4; (28) x2+1/3, x1+2/3, −x3+2/3, −x4; (29) x1x2+1/3, −x2+2/3, −x3+2/3, −x4; (30) −x1+1/3, −x1+x2+2/3, −x3+2/3, −x4; (31) −x1+1/3, −x2+2/3, −x3+2/3, −x4; (32) x2+1/3, −x1+x2+2/3, −x3+2/3, −x4; (33) x1x2+1/3, x1+2/3, −x3+2/3, −x4; (34) −x2+1/3, −x1+2/3, x3+2/3, x4; (35) −x1+x2+1/3, x2+2/3, x3+2/3, x4; (36) x1+1/3, x1x2+2/3, x3+2/3, x4.

Data collection top
2θmin = 5.5°, 2θmax = 42.1°, 2θstep = 0.01°
Refinement top
Rp = 0.02168 parameters
Rwp = 0.0300 restraints
Rexp = 0.0304 constraints
R(F) = 0.016Weighting scheme based on measured s.u.'s
χ2 = 1.000(Δ/σ)max = 5.113
3661 data pointsBackground function: 36 Legendre polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: March & Dollase
Crystal data top
Sb0.89Te0.11V = 90.75 (1) Å3
Mr = 122.4Z = 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) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x1+x2, −x1, x3, x4; (4) x2, x1, −x3, −x4; (5) x1x2, −x2, −x3, −x4; (6) −x1, −x1+x2, −x3, −x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x1x2, x1, −x3, −x4; (10) −x2, −x1, x3, x4; (11) −x1+x2, x2, x3, x4; (12) x1, x1x2, x3, x4; (13) x1+2/3, x2+1/3, x3+1/3, x4; (14) −x2+2/3, x1x2+1/3, x3+1/3, x4; (15) −x1+x2+2/3, −x1+1/3, x3+1/3, x4; (16) x2+2/3, x1+1/3, −x3+1/3, −x4; (17) x1x2+2/3, −x2+1/3, −x3+1/3, −x4; (18) −x1+2/3, −x1+x2+1/3, −x3+1/3, −x4; (19) −x1+2/3, −x2+1/3, −x3+1/3, −x4; (20) x2+2/3, −x1+x2+1/3, −x3+1/3, −x4; (21) x1x2+2/3, x1+1/3, −x3+1/3, −x4; (22) −x2+2/3, −x1+1/3, x3+1/3, x4; (23) −x1+x2+2/3, x2+1/3, x3+1/3, x4; (24) x1+2/3, x1x2+1/3, x3+1/3, x4; (25) x1+1/3, x2+2/3, x3+2/3, x4; (26) −x2+1/3, x1x2+2/3, x3+2/3, x4; (27) −x1+x2+1/3, −x1+2/3, x3+2/3, x4; (28) x2+1/3, x1+2/3, −x3+2/3, −x4; (29) x1x2+1/3, −x2+2/3, −x3+2/3, −x4; (30) −x1+1/3, −x1+x2+2/3, −x3+2/3, −x4; (31) −x1+1/3, −x2+2/3, −x3+2/3, −x4; (32) x2+1/3, −x1+x2+2/3, −x3+2/3, −x4; (33) x1x2+1/3, x1+2/3, −x3+2/3, −x4; (34) −x2+1/3, −x1+2/3, x3+2/3, x4; (35) −x1+x2+1/3, x2+2/3, x3+2/3, x4; (36) x1+1/3, x1x2+2/3, x3+2/3, x4.

Data collection top
2θmin = 5.5°, 2θmax = 42.1°, 2θstep = 0.01°
Refinement top
Rp = 0.0213661 data points
Rwp = 0.03068 parameters
Rexp = 0.0300 restraints
R(F) = 0.016(Δ/σ)max = 5.113
χ2 = 1.000
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sb10000.0116 (3)0.887
Te10000.0116 (3)0.113
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.0123 (2)0.0123 (2)0.0101 (7)0.00614 (12)00
Te10.0123 (2)0.0122850.0101 (7)0.00614300
(III) top
Crystal data top
AgInTe2Z = 4
Mr = 477.9F(000) = 800
Tetragonal, I42dDx = 6.092 Mg m3
Hall symbol: I -4;2bw? radiation, λ = 0.41873 Å
a = 6.4275 (3) ÅT = 293 K
c = 12.6089 (9) Å?, ? × ? × ? mm
V = 520.91 (5) Å3
Data collection top
2θmin = 5.5°, 2θmax = 42.1°, 2θstep = 0.01°
Refinement top
Rp = 0.02168 parameters
Rwp = 0.0300 restraints
Rexp = 0.0304 constraints
R(F) = 0.016Weighting scheme based on measured s.u.'s
χ2 = 1.000(Δ/σ)max = 5.113
3661 data pointsBackground function: 36 Legendre polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: none
Crystal data top
AgInTe2V = 520.91 (5) Å3
Mr = 477.9Z = 4
Tetragonal, I42d? radiation, λ = 0.41873 Å
a = 6.4275 (3) ÅT = 293 K
c = 12.6089 (9) Å?, ? × ? × ? mm
Data collection top
2θmin = 5.5°, 2θmax = 42.1°, 2θstep = 0.01°
Refinement top
Rp = 0.0213661 data points
Rwp = 0.03068 parameters
Rexp = 0.0300 restraints
R(F) = 0.016(Δ/σ)max = 5.113
χ2 = 1.000
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ag1000.50.0289 (13)*
In10000.0289 (13)*
Te20.252 (11)0.250.1250.0289 (13)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
(IV) top
Crystal data top
Sb0.87Te0.13Z = 3
Mr = 122.5F(000) = 1841
Trigonal, R3m(00γ)00†Dx = 6.598 Mg m3
q = 1.56522c*X-ray radiation, λ = 0.41853 Å
a = 4.3181 ÅT = 773 K
c = 5.7267 Å?, ? × ? × ? mm
V = 92.47 Å3
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x2, −x1, x3, x4; (4) −x1+x2, −x1, x3, x4; (5) x1, x1x2, x3, x4; (6) −x1+x2, x2, x3, x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x2, x1, −x3, −x4; (10) x1x2, x1, −x3, −x4; (11) −x1, −x1+x2, −x3, −x4; (12) x1x2, −x2, −x3, −x4; (13) 2/3+x1, 1/3+x2, 1/3+x3, x4; (14) 2/3−x2, 1/3+x1x2, 1/3+x3, x4; (15) 2/3−x2, 1/3−x1, 1/3+x3, x4; (16) 2/3−x1+x2, 1/3−x1, 1/3+x3, x4; (17) 2/3+x1, 1/3+x1x2, 1/3+x3, x4; (18) 2/3−x1+x2, 1/3+x2, 1/3+x3, x4; (19) 2/3−x1, 1/3−x2, 1/3−x3, −x4; (20) 2/3+x2, 1/3−x1+x2, 1/3−x3, −x4; (21) 2/3+x2, 1/3+x1, 1/3−x3, −x4; (22) 2/3+x1x2, 1/3+x1, 1/3−x3, −x4; (23) 2/3−x1, 1/3−x1+x2, 1/3−x3, −x4; (24) 2/3+x1x2, 1/3−x2, 1/3−x3, −x4; (25) 1/3+x1, 2/3+x2, 2/3+x3, x4; (26) 1/3−x2, 2/3+x1x2, 2/3+x3, x4; (27) 1/3−x2, 2/3−x1, 2/3+x3, x4; (28) 1/3−x1+x2, 2/3−x1, 2/3+x3, x4; (29) 1/3+x1, 2/3+x1x2, 2/3+x3, x4; (30) 1/3−x1+x2, 2/3+x2, 2/3+x3, x4; (31) 1/3−x1, 2/3−x2, 2/3−x3, −x4; (32) 1/3+x2, 2/3−x1+x2, 2/3−x3, −x4; (33) 1/3+x2, 2/3+x1, 2/3−x3, −x4; (34) 1/3+x1x2, 2/3+x1, 2/3−x3, −x4; (35) 1/3−x1, 2/3−x1+x2, 2/3−x3, −x4; (36) 1/3+x1x2, 2/3−x2, 2/3−x3, −x4.

Data collection top
2θmin = 3.02°, 2θmax = 30.5°, 2θstep = 0.02°
Refinement top
Rp = 0.020Profile function: Pseudo-Voigt
Rwp = 0.02959 parameters
Rexp = 0.024Weighting scheme based on measured s.u.'s
R(F) = 0.030(Δ/σ)max = 0.628
χ2 = NOT FOUNDBackground function: 36 Legendre polynoms
1375 data pointsPreferred orientation correction: none
Crystal data top
Sb0.87Te0.13V = 92.47 Å3
Mr = 122.5Z = 3
Trigonal, R3m(00γ)00†X-ray radiation, λ = 0.41853 Å
q = 1.56522c*T = 773 K
a = 4.3181 Å?, ? × ? × ? mm
c = 5.7267 Å
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x2, −x1, x3, x4; (4) −x1+x2, −x1, x3, x4; (5) x1, x1x2, x3, x4; (6) −x1+x2, x2, x3, x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x2, x1, −x3, −x4; (10) x1x2, x1, −x3, −x4; (11) −x1, −x1+x2, −x3, −x4; (12) x1x2, −x2, −x3, −x4; (13) 2/3+x1, 1/3+x2, 1/3+x3, x4; (14) 2/3−x2, 1/3+x1x2, 1/3+x3, x4; (15) 2/3−x2, 1/3−x1, 1/3+x3, x4; (16) 2/3−x1+x2, 1/3−x1, 1/3+x3, x4; (17) 2/3+x1, 1/3+x1x2, 1/3+x3, x4; (18) 2/3−x1+x2, 1/3+x2, 1/3+x3, x4; (19) 2/3−x1, 1/3−x2, 1/3−x3, −x4; (20) 2/3+x2, 1/3−x1+x2, 1/3−x3, −x4; (21) 2/3+x2, 1/3+x1, 1/3−x3, −x4; (22) 2/3+x1x2, 1/3+x1, 1/3−x3, −x4; (23) 2/3−x1, 1/3−x1+x2, 1/3−x3, −x4; (24) 2/3+x1x2, 1/3−x2, 1/3−x3, −x4; (25) 1/3+x1, 2/3+x2, 2/3+x3, x4; (26) 1/3−x2, 2/3+x1x2, 2/3+x3, x4; (27) 1/3−x2, 2/3−x1, 2/3+x3, x4; (28) 1/3−x1+x2, 2/3−x1, 2/3+x3, x4; (29) 1/3+x1, 2/3+x1x2, 2/3+x3, x4; (30) 1/3−x1+x2, 2/3+x2, 2/3+x3, x4; (31) 1/3−x1, 2/3−x2, 2/3−x3, −x4; (32) 1/3+x2, 2/3−x1+x2, 2/3−x3, −x4; (33) 1/3+x2, 2/3+x1, 2/3−x3, −x4; (34) 1/3+x1x2, 2/3+x1, 2/3−x3, −x4; (35) 1/3−x1, 2/3−x1+x2, 2/3−x3, −x4; (36) 1/3+x1x2, 2/3−x2, 2/3−x3, −x4.

Data collection top
2θmin = 3.02°, 2θmax = 30.5°, 2θstep = 0.02°
Refinement top
Rp = 0.020χ2 = NOT FOUND
Rwp = 0.0291375 data points
Rexp = 0.02459 parameters
R(F) = 0.030(Δ/σ)max = 0.628
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sb10000.03832 (14)0.870
Te10000.03832 (12)0.130
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.03681 (14)0.03681 (14)0.0413 (3)0.01841 (7)00
Te10.03681 (14)0.036810.0413 (3)0.01840500
Bond lengths (Å) top
AverageMinimumMaximum
Sb1—Sb1i3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1ii3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1iii3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1iv3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1v3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1vi3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Te1i3.1483 (6)2.8798 (9)3.4307 (9)
Sb1—Te1ii3.1483 (6)2.8798 (9)3.4307 (9)
Sb1—Te1iii3.1483 (6)2.8798 (9)3.4307 (9)
Sb1—Te1iv3.1491 (6)2.8804 (9)3.4316 (9)
Sb1—Te1v3.1491 (6)2.8804 (9)3.4316 (9)
Sb1—Te1vi3.1491 (6)2.8804 (9)3.4316 (9)
Symmetry codes: (i) x11/3, x22/3, x3+1/3, x4; (ii) x11/3, x2+1/3, x3+1/3, x4; (iii) x1+2/3, x2+1/3, x3+1/3, x4; (iv) x12/3, x21/3, x31/3, x4; (v) x1+1/3, x21/3, x31/3, x4; (vi) x1+1/3, x2+2/3, x31/3, x4.
(V) top
Crystal data top
Sb2O3Z = 16
Mr = 291.5F(000) = 1841
Cubic, Fd3mDx = 5.442 Mg m3
Hall symbol: -F 4vw;2vw;3X-ray radiation, λ = 0.41853 Å
a = 11.2471 ÅT = 773 K
V = 1422.71 Å3?, ? × ? × ? mm
Data collection top
2θmin = 3.02°, 2θmax = 30.5°, 2θstep = 0.02°
Refinement top
Rp = 0.020Profile function: Pseudo-Voigt
Rwp = 0.02959 parameters
Rexp = 0.024Weighting scheme based on measured s.u.'s
R(F) = 0.030(Δ/σ)max = 0.628
χ2 = NOT FOUNDBackground function: 36 Legendre polynoms
1375 data pointsPreferred orientation correction: none
Crystal data top
Sb2O3Z = 16
Mr = 291.5X-ray radiation, λ = 0.41853 Å
Cubic, Fd3mT = 773 K
a = 11.2471 Å?, ? × ? × ? mm
V = 1422.71 Å3
Data collection top
2θmin = 3.02°, 2θmax = 30.5°, 2θstep = 0.02°
Refinement top
Rp = 0.020χ2 = NOT FOUND
Rwp = 0.0291375 data points
Rexp = 0.02459 parameters
R(F) = 0.030(Δ/σ)max = 0.628
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sb20.88704 (13)0.88704 (13)0.88704 (13)0.0264 (14)*
O10.188 (2)000.0264 (14)*
Bond lengths (Å) top
Sb2—O1i1.986 (10)O1—O1viii2.99 (2)
Sb2—O1ii2.936 (16)O1—O1ix2.979 (8)
Sb2—O1iii2.936 (16)O1—O1x2.99 (2)
Sb2—O1iv1.986 (10)O1—O1xi2.979 (8)
Sb2—O1v2.936 (16)O1—O1xii2.99 (2)
Sb2—O1vi1.986 (10)O1—O1xiii2.979 (8)
O1—O1vii2.979 (8)O1—O1xiv2.99 (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, x1/4, z1/4; (viii) z, x, y; (ix) y+1/4, x+1/4, z+1/4; (x) z, x, y; (xi) z+1/4, y1/4, x1/4; (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 formulaAg0.034In0.037Sb0.764Te0.165Sb0.89Te0.11AgInTe2Sb0.87Te0.13
Mr122122.4477.9122.5
Crystal system, space groupTrigonal, R3m(00γ)00†Trigonal, R3m(00γ)00‡Tetragonal, I42dTrigonal, R3m(00γ)00§
Temperature (K)545293293773
Wave vectorsq = 1.500000c*q = 1.551587c*I -4;2bwq = 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, 904.3181, 4.3181, 5.7267
α, β, γ (°)90, 90, 12090, 90, 120520.91 (5)90, 90, 120
V3)90.55 (2)90.75 (1)492.47
Z338003
Radiation type?, λ = 0.41873 Å?, λ = 0.41873 ÅX-ray, λ = 0.41853 Å
µ (mm1)?
Specimen shape, size (mm)?, ? × ? × ??, ? × ? × ??, ? × ? × ?
Data collection
Diffractometer????
Specimen mounting????
Data collection mode????
Scan method????
2θ values (°)2θmin = 5.5 2θmax = 31.5 2θstep = 0.012θmin = 5.5 2θmax = 42.1 2θstep = 0.012θmin = 5.5 2θmax = 42.1 2θstep = 0.012θmin = 3.02 2θmax = 30.5 2θstep = 0.02
Refinement
R factors and goodness of fitRp = 0.020, Rwp = 0.029, Rexp = 0.030, R(F) = 0.013, χ2 = 0.960Rp = 0.021, Rwp = 0.030, Rexp = 0.030, R(F) = 0.016, χ2 = 1.000Rp = 0.021, Rwp = 0.030, Rexp = 0.030, R(F) = 0.016, χ2 = 1.000Rp = 0.020, Rwp = 0.029, Rexp = 0.024, R(F) = 0.030, χ2 = NOT FOUND
No. of data points2601366136611375
No. of parameters56686859
No. of restraints000?
(Δ/σ)max7.0615.1135.1130.628


(V)
Crystal data
Chemical formulaSb2O3
Mr291.5
Crystal system, space groupCubic, Fd3m
Temperature (K)773
Wave vectors-F 4vw;2vw;3
a, b, c (Å)90, 90, 90
α, β, γ (°)1422.71
V3)16
Z1841
Radiation type
µ (mm1)?
Specimen shape, size (mm)
Data collection
Diffractometer?
Specimen mounting?
Data collection mode?
Scan method?
2θ values (°)2θmin = 3.02 2θmax = 30.5 2θstep = 0.02
Refinement
R factors and goodness of fitRp = 0.020, Rwp = 0.029, Rexp = 0.024, R(F) = 0.030, χ2 = NOT FOUND
No. of data points1375
No. of parameters59
No. of restraints?
(Δ/σ)max0.628

† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x1+x2, −x1, x3, x4; (4) x2, x1, −x3, −x4; (5) x1x2, −x2, −x3, −x4; (6) −x1, −x1+x2, −x3, −x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x1x2, x1, −x3, −x4; (10) −x2, −x1, x3, x4; (11) −x1+x2, x2, x3, x4; (12) x1, x1x2, x3, x4; (13) x1+2/3, x2+1/3, x3+1/3, x4; (14) −x2+2/3, x1x2+1/3, x3+1/3, x4; (15) −x1+x2+2/3, −x1+1/3, x3+1/3, x4; (16) x2+2/3, x1+1/3, −x3+1/3, −x4; (17) x1x2+2/3, −x2+1/3, −x3+1/3, −x4; (18) −x1+2/3, −x1+x2+1/3, −x3+1/3, −x4; (19) −x1+2/3, −x2+1/3, −x3+1/3, −x4; (20) x2+2/3, −x1+x2+1/3, −x3+1/3, −x4; (21) x1x2+2/3, x1+1/3, −x3+1/3, −x4; (22) −x2+2/3, −x1+1/3, x3+1/3, x4; (23) −x1+x2+2/3, x2+1/3, x3+1/3, x4; (24) x1+2/3, x1x2+1/3, x3+1/3, x4; (25) x1+1/3, x2+2/3, x3+2/3, x4; (26) −x2+1/3, x1x2+2/3, x3+2/3, x4; (27) −x1+x2+1/3, −x1+2/3, x3+2/3, x4; (28) x2+1/3, x1+2/3, −x3+2/3, −x4; (29) x1x2+1/3, −x2+2/3, −x3+2/3, −x4; (30) −x1+1/3, −x1+x2+2/3, −x3+2/3, −x4; (31) −x1+1/3, −x2+2/3, −x3+2/3, −x4; (32) x2+1/3, −x1+x2+2/3, −x3+2/3, −x4; (33) x1x2+1/3, x1+2/3, −x3+2/3, −x4; (34) −x2+1/3, −x1+2/3, x3+2/3, x4; (35) −x1+x2+1/3, x2+2/3, x3+2/3, x4; (36) x1+1/3, x1x2+2/3, x3+2/3, x4.

‡ Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x1+x2, −x1, x3, x4; (4) x2, x1, −x3, −x4; (5) x1x2, −x2, −x3, −x4; (6) −x1, −x1+x2, −x3, −x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x1x2, x1, −x3, −x4; (10) −x2, −x1, x3, x4; (11) −x1+x2, x2, x3, x4; (12) x1, x1x2, x3, x4; (13) x1+2/3, x2+1/3, x3+1/3, x4; (14) −x2+2/3, x1x2+1/3, x3+1/3, x4; (15) −x1+x2+2/3, −x1+1/3, x3+1/3, x4; (16) x2+2/3, x1+1/3, −x3+1/3, −x4; (17) x1x2+2/3, −x2+1/3, −x3+1/3, −x4; (18) −x1+2/3, −x1+x2+1/3, −x3+1/3, −x4; (19) −x1+2/3, −x2+1/3, −x3+1/3, −x4; (20) x2+2/3, −x1+x2+1/3, −x3+1/3, −x4; (21) x1x2+2/3, x1+1/3, −x3+1/3, −x4; (22) −x2+2/3, −x1+1/3, x3+1/3, x4; (23) −x1+x2+2/3, x2+1/3, x3+1/3, x4; (24) x1+2/3, x1x2+1/3, x3+1/3, x4; (25) x1+1/3, x2+2/3, x3+2/3, x4; (26) −x2+1/3, x1x2+2/3, x3+2/3, x4; (27) −x1+x2+1/3, −x1+2/3, x3+2/3, x4; (28) x2+1/3, x1+2/3, −x3+2/3, −x4; (29) x1x2+1/3, −x2+2/3, −x3+2/3, −x4; (30) −x1+1/3, −x1+x2+2/3, −x3+2/3, −x4; (31) −x1+1/3, −x2+2/3, −x3+2/3, −x4; (32) x2+1/3, −x1+x2+2/3, −x3+2/3, −x4; (33) x1x2+1/3, x1+2/3, −x3+2/3, −x4; (34) −x2+1/3, −x1+2/3, x3+2/3, x4; (35) −x1+x2+1/3, x2+2/3, x3+2/3, x4; (36) x1+1/3, x1x2+2/3, x3+2/3, x4.

§ Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1x2, x3, x4; (3) −x2, −x1, x3, x4; (4) −x1+x2, −x1, x3, x4; (5) x1, x1x2, x3, x4; (6) −x1+x2, x2, x3, x4; (7) −x1, −x2, −x3, −x4; (8) x2, −x1+x2, −x3, −x4; (9) x2, x1, −x3, −x4; (10) x1x2, x1, −x3, −x4; (11) −x1, −x1+x2, −x3, −x4; (12) x1x2, −x2, −x3, −x4; (13) 2/3+x1, 1/3+x2, 1/3+x3, x4; (14) 2/3−x2, 1/3+x1x2, 1/3+x3, x4; (15) 2/3−x2, 1/3−x1, 1/3+x3, x4; (16) 2/3−x1+x2, 1/3−x1, 1/3+x3, x4; (17) 2/3+x1, 1/3+x1x2, 1/3+x3, x4; (18) 2/3−x1+x2, 1/3+x2, 1/3+x3, x4; (19) 2/3−x1, 1/3−x2, 1/3−x3, −x4; (20) 2/3+x2, 1/3−x1+x2, 1/3−x3, −x4; (21) 2/3+x2, 1/3+x1, 1/3−x3, −x4; (22) 2/3+x1x2, 1/3+x1, 1/3−x3, −x4; (23) 2/3−x1, 1/3−x1+x2, 1/3−x3, −x4; (24) 2/3+x1x2, 1/3−x2, 1/3−x3, −x4; (25) 1/3+x1, 2/3+x2, 2/3+x3, x4; (26) 1/3−x2, 2/3+x1x2, 2/3+x3, x4; (27) 1/3−x2, 2/3−x1, 2/3+x3, x4; (28) 1/3−x1+x2, 2/3−x1, 2/3+x3, x4; (29) 1/3+x1, 2/3+x1x2, 2/3+x3, x4; (30) 1/3−x1+x2, 2/3+x2, 2/3+x3, x4; (31) 1/3−x1, 2/3−x2, 2/3−x3, −x4; (32) 1/3+x2, 2/3−x1+x2, 2/3−x3, −x4; (33) 1/3+x2, 2/3+x1, 2/3−x3, −x4; (34) 1/3+x1x2, 2/3+x1, 2/3−x3, −x4; (35) 1/3−x1, 2/3−x1+x2, 2/3−x3, −x4; (36) 1/3+x1x2, 2/3−x2, 2/3−x3, −x4.

Computer programs: Jana2000 (Petricek, Dusek & Palatinus, 2000).

Selected bond lengths (Å) for (IV) top
AverageMinimumMaximum
Sb1—Sb1i3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1ii3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1iii3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1iv3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1v3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Sb1vi3.1499 (14)2.9339 (7)3.3530 (8)
Sb1—Te1i3.1483 (6)2.8798 (9)3.4307 (9)
Sb1—Te1ii3.1483 (6)2.8798 (9)3.4307 (9)
Sb1—Te1iii3.1483 (6)2.8798 (9)3.4307 (9)
Sb1—Te1iv3.1491 (6)2.8804 (9)3.4316 (9)
Sb1—Te1v3.1491 (6)2.8804 (9)3.4316 (9)
Sb1—Te1vi3.1491 (6)2.8804 (9)3.4316 (9)
Symmetry codes: (i) x11/3, x22/3, x3+1/3, x4; (ii) x11/3, x2+1/3, x3+1/3, x4; (iii) x1+2/3, x2+1/3, x3+1/3, x4; (iv) x12/3, x21/3, x31/3, x4; (v) x1+1/3, x21/3, x31/3, x4; (vi) x1+1/3, x2+2/3, x31/3, x4.
Selected bond lengths (Å) for (V) top
Sb2—O1i1.986 (10)O1—O1viii2.99 (2)
Sb2—O1ii2.936 (16)O1—O1ix2.979 (8)
Sb2—O1iii2.936 (16)O1—O1x2.99 (2)
Sb2—O1iv1.986 (10)O1—O1xi2.979 (8)
Sb2—O1v2.936 (16)O1—O1xii2.99 (2)
Sb2—O1vi1.986 (10)O1—O1xiii2.979 (8)
O1—O1vii2.979 (8)O1—O1xiv2.99 (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, x1/4, z1/4; (viii) z, x, y; (ix) y+1/4, x+1/4, z+1/4; (x) z, x, y; (xi) z+1/4, y1/4, x1/4; (xii) y, z, x; (xiii) z+1/4, y+1/4, x+1/4; (xiv) y, z, x.
 

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