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Acta Cryst. (2011). B67, 381-385
https://doi.org/10.1107/S0108768111033738
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Crystallization of the chalcogenide compound Sb8Te3

K. Kifune, T. Fujita, Y. Kubota, N. Yamada and T. Matsunaga
The crystallization of a sputtered Sb8Te3 film was examined in an X-ray powder diffraction experiment. An as-sputtered, amorphous Sb8Te3 film crystallized during heating into a structure of Sb–Te homologous series modulated along the stacking direction. During heating the lattice parameters and the modulation period γ were found to change significantly and continuously; this observation suggests a continuous change in the stacking sequence. A superspace analysis revealed that with heating the modulation period γ increased to a value that seemed to be determined by the atomic composition. Once γ reached this value it remained unchanged with cooling. A three-dimensional projection of the converged four-dimensional superspace structure corresponded to the homologous Sb8Te3 structure.
Keywords: chalcogenide compound; phase change; homologous structure.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768111033738/so5052sup1.cif
Contains datablocks global, (I)

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768111033738/so5052Isup2.rtv
Contains datablock I

Computing details top

Program(s) used to refine structure: Jana2000 (Petricek, Dusek & Palatinus, 2000); software used to prepare material for publication: Jana2000 (Petricek, Dusek & Palatinus, 2000).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(I) top
Crystal data top
Sb8Te3Z = 1
Mr = 1356.8F(000) = 1846
Trigonal, R3m(00γ)†Dx = 23.831 Mg m−3
q = 1.63774c*Synchrotron radiation, λ = 0.4209 Å
a = 4.3134 ŵ = 18.43 mm−1
c = 5.8658 ÅT = 831 K
V = 94.51 Å3cylinder, 3.0 × 0.3 mm
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1−x2, x3, x4; (3) −x2, −x1, x3, x4; (4) −x1+x2, −x1, x3, x4; (5) x1, x1−x2, 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) x1−x2, x1, −x3, −x4; (11) −x1, −x1+x2, −x3, −x4; (12) x1−x2, −x2, −x3, −x4; (13) 2/3+x1, 1/3+x2, 1/3+x3, x4; (14) 2/3−x2, 1/3+x1−x2, 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+x1−x2, 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+x1−x2, 1/3+x1, 1/3−x3, −x4; (23) 2/3−x1, 1/3−x1+x2, 1/3−x3, −x4; (24) 2/3+x1−x2, 1/3−x2, 1/3−x3, −x4; (25) 1/3+x1, 2/3+x2, 2/3+x3, x4; (26) 1/3−x2, 2/3+x1−x2, 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+x1−x2, 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+x1−x2, 2/3+x1, 2/3−x3, −x4; (35) 1/3−x1, 2/3−x1+x2, 2/3−x3, −x4; (36) 1/3+x1−x2, 2/3−x2, 2/3−x3, −x4.

Data collection top
Debye-Scherrer camera
diffractometer		Data collection mode: transmission
Si 111 monochromatorScan method: Stationary detector
Specimen mounting: sealed quartz capillary tube
Refinement top
Rp = 0.03251 parameters
Rwp = 0.0460 restraints
Rexp = 0.0240 constraints
R(F) = 0.062Weighting scheme based on measured s.u.'s
χ2 = NOT FOUND(Δ/σ)max = 0.481
3781 data pointsBackground function: 36 Legendre polynoms
Profile function: Pseudo-VoigtPreferred orientation correction: March & Dollase
Crystal data top
Sb8Te3V = 94.51 Å3
Mr = 1356.8Z = 1
Trigonal, R3m(00γ)†Synchrotron radiation, λ = 0.4209 Å
q = 1.63774c*µ = 18.43 mm−1
a = 4.3134 ÅT = 831 K
c = 5.8658 Åcylinder, 3.0 × 0.3 mm
† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1−x2, x3, x4; (3) −x2, −x1, x3, x4; (4) −x1+x2, −x1, x3, x4; (5) x1, x1−x2, 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) x1−x2, x1, −x3, −x4; (11) −x1, −x1+x2, −x3, −x4; (12) x1−x2, −x2, −x3, −x4; (13) 2/3+x1, 1/3+x2, 1/3+x3, x4; (14) 2/3−x2, 1/3+x1−x2, 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+x1−x2, 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+x1−x2, 1/3+x1, 1/3−x3, −x4; (23) 2/3−x1, 1/3−x1+x2, 1/3−x3, −x4; (24) 2/3+x1−x2, 1/3−x2, 1/3−x3, −x4; (25) 1/3+x1, 2/3+x2, 2/3+x3, x4; (26) 1/3−x2, 2/3+x1−x2, 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+x1−x2, 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+x1−x2, 2/3+x1, 2/3−x3, −x4; (35) 1/3−x1, 2/3−x1+x2, 2/3−x3, −x4; (36) 1/3+x1−x2, 2/3−x2, 2/3−x3, −x4.

Data collection top
Debye-Scherrer camera
diffractometer		Data collection mode: transmission
Specimen mounting: sealed quartz capillary tubeScan method: Stationary detector
Refinement top
Rp = 0.0323781 data points
Rwp = 0.04651 parameters
Rexp = 0.0240 restraints
R(F) = 0.062(Δ/σ)max = 0.481
χ2 = NOT FOUND
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sb10000.0551 (4)*0.724
Te10000.0294 (5)*0.276
Bond lengths (Å) top
AverageMinimumMaximum
Sb1—Sb1i3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1ii3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1iii3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1iv3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1v3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1vi3.1402 (12)2.8867 (12)3.4938 (17)
Symmetry codes: (i) x1−1/3, x2−2/3, x3+1/3, x4; (ii) x1−1/3, x2+1/3, x3+1/3, x4; (iii) x1+2/3, x2+1/3, x3+1/3, x4; (iv) x1−2/3, x2−1/3, x3−1/3, x4; (v) x1+1/3, x2−1/3, x3−1/3, x4; (vi) x1+1/3, x2+2/3, x3−1/3, x4.

Experimental details

Crystal data
Chemical formulaSb8Te3
Mr1356.8
Crystal system, space groupTrigonal, R3m(00γ)†
Temperature (K)831
Wave vectorsq = 1.63774c*
a, c (Å)4.3134, 5.8658
V (Å3)94.51
Z1
Radiation typeSynchrotron, λ = 0.4209 Å
µ (mm−1)18.43
Specimen shape, size (mm)Cylinder, 3.0 × 0.3
Data collection
DiffractometerDebye-Scherrer camera
diffractometer
Specimen mountingSealed quartz capillary tube
Data collection modeTransmission
Scan methodStationary detector
2θ values (°)2θfixed = ?
Refinement
R factors and goodness of fitRp = 0.032, Rwp = 0.046, Rexp = 0.024, R(F) = 0.062, χ2 = NOT FOUND
No. of data points3781
No. of parameters51
(Δ/σ)max0.481

† Symmetry operations: (1) x1, x2, x3, x4; (2) −x2, x1−x2, x3, x4; (3) −x2, −x1, x3, x4; (4) −x1+x2, −x1, x3, x4; (5) x1, x1−x2, 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) x1−x2, x1, −x3, −x4; (11) −x1, −x1+x2, −x3, −x4; (12) x1−x2, −x2, −x3, −x4; (13) 2/3+x1, 1/3+x2, 1/3+x3, x4; (14) 2/3−x2, 1/3+x1−x2, 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+x1−x2, 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+x1−x2, 1/3+x1, 1/3−x3, −x4; (23) 2/3−x1, 1/3−x1+x2, 1/3−x3, −x4; (24) 2/3+x1−x2, 1/3−x2, 1/3−x3, −x4; (25) 1/3+x1, 2/3+x2, 2/3+x3, x4; (26) 1/3−x2, 2/3+x1−x2, 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+x1−x2, 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+x1−x2, 2/3+x1, 2/3−x3, −x4; (35) 1/3−x1, 2/3−x1+x2, 2/3−x3, −x4; (36) 1/3+x1−x2, 2/3−x2, 2/3−x3, −x4.

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

Selected bond lengths (Å) top
AverageMinimumMaximum
Sb1—Sb1i3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1ii3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1iii3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1iv3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1v3.1402 (12)2.8867 (12)3.4938 (17)
Sb1—Sb1vi3.1402 (12)2.8867 (12)3.4938 (17)
Symmetry codes: (i) x1−1/3, x2−2/3, x3+1/3, x4; (ii) x1−1/3, x2+1/3, x3+1/3, x4; (iii) x1+2/3, x2+1/3, x3+1/3, x4; (iv) x1−2/3, x2−1/3, x3−1/3, x4; (v) x1+1/3, x2−1/3, x3−1/3, x4; (vi) x1+1/3, x2+2/3, x3−1/3, x4.
 

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