Thermal stability of the layered modification of Cu0.5ZrTe2 in the temperature range 25–900 °C

Shkvarina, E.G.; Titov, A.A.; Shkvarin, A.S.; Plaisier, J.R.; Gigli, L.; Titov, A.N.

doi:10.1107/S2053229618009841

Thermal stability of the layered modification of Cu_0.5ZrTe₂ in the temperature range 25–900 °C

E. G. Shkvarina, A. A. Titov, A. S. Shkvarin, J. R. Plaisier, L. Gigli and A. N. Titov

The thermal stability of the layered modification of the Cu_0.5ZrTe₂ polycrystalline intercalation compound, synthesized at room temperature, has been studied in the temperature range 25–900 °C. A change in the occupation of the octahedral and tetrahedral coordinated sites in the interlayer space of the zirconium ditelluride was observed using in-situ time-resolved synchrotron X-ray powder diffraction experiments. The formation of the rhombohedral CuZr₂Te₄ phase, which is stable in the temperature range 300–700 °C, has been observed. The copper intercalation at room temperature leads to the formation of a phase in which the Cu atoms occupy only octahedral sites in the interlayer space. At temperatures above the decay temperature of the rhombohedral CuZr₂Te₄, a layered phase with Cu atoms uniformly distributed between octahedral and tetrahedral sites in the interlayer space is stable. The changes in the crystal structure independent of temperature are in agreement with the previously proposed model, according to which the stability of the layered or the rhombohedral phase is determined by the entropy factor associated with the distribution of the intercalated atoms between the octahedral and tetrahedral sites in the interlayer space.

Keywords: powder diffraction; thermal stability; copper intercalation; zirconium; tellurium; layered modification; polycrystalline compound; synchrotron; time resolved; GSAS.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009841/qs3073sup1.cif Contains datablocks SINCU05ZRTE2_overall, global, SINCU05ZRTE2_phase_1, SINCU05ZRTE2_phase_2, SINCU05ZRTE2_phase_3, SINCU05ZRTE2_phase_4
	Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618009841/qs3073sup2.pdf Additional figures
	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009841/qs3073sup3.cif Cif file for Cu0.5ZrTe2 2 at 500C
	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009841/qs3073sup4.cif Cif file for Cu0.5ZrTe2 2 at 900C
	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009841/qs3073sup5.cif Cif file for Cu0.5ZrTe2 2 after annealing at 467C for one week
	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009841/qs3073sup6.cif Cif file for Cu0.5ZrTe2 2 at RT
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S2053229618009841/qs3073sup7.rtv Contains datablock WISH_publ
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229618009841/qs3073sup8.hkl Contains datablock WISH_publ

CCDC references: 1854888; 1854887; 1854886; 1854885

Computing details top

(SINCU05ZRTE2_phase_1) top

Crystal data top

Cu2.47Te8Zr4	c = 13.2455 (8) Å
M_r = 771.43	β = 89.969 (14)°
Monoclinic, I2/m	V = 357.59 (9) Å³
Hall symbol: -I 2y	Z = 2
a = 6.8317 (15) Å	Cu Kα radiation
b = 3.9517 (3) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Zr2	−0.02546	0.0	0.25138	0.05587
Te3	0.1872	0.5	0.88172	0.03302
Te4	0.3222	0.0	0.11922	−0.00557
CU5	0.0	0.0	0.5	0.57145*
CU7	0.0	0.0	0.0	0.07773*	0.23674

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zr2	0.25757	−0.08361	−0.0063	0.0	−0.05163	0.0
Te3	0.11932	−0.08039	0.06024	0.0	−0.11154	0.0
Te4	0.01293	−0.04553	0.01596	0.0	−0.07089	0.0

Geometric parameters (Å, º) top

Zr2—Te3ⁱ	2.8697 (2)	Te4—CU5^x	2.8055 (2)
Zr2—Te3ⁱⁱ	2.8697 (2)	Te4—CU5^xi	2.8055 (2)
Zr2—Te3ⁱⁱⁱ	2.6135 (5)	Te4—CU7	2.7097 (5)
Zr2—Te4	2.9498 (5)	CU5—Te3ⁱⁱⁱ	2.6504 (5)
Zr2—Te4^iv	2.9619 (3)	CU5—Te3^xii	2.6504 (5)
Zr2—Te4^v	2.9619 (3)	CU5—Te4^xiii	2.8055 (2)
Te3—Zr2ⁱⁱ	2.8697 (2)	CU5—Te4^xiv	2.8055 (2)
Te3—Zr2^vi	2.8697 (2)	CU5—Te4^iv	2.8055 (2)
Te3—Zr2^vii	2.6135 (5)	CU5—Te4^v	2.8055 (2)
Te3—CU5^vii	2.6504 (5)	CU7—Te3^xv	2.8270 (2)
Te3—CU7^viii	2.8270 (2)	CU7—Te3^xvi	2.8270 (2)
Te3—CU7^ix	2.8270 (2)	CU7—Te3ⁱ	2.8270 (2)
Te4—Zr2	2.9498 (5)	CU7—Te3ⁱⁱ	2.8270 (2)
Te4—Zr2^iv	2.9619 (3)	CU7—Te4	2.7097 (5)
Te4—Zr2^v	2.9619 (3)	CU7—Te4^xvii	2.7097 (5)

Te3ⁱ—Zr2—Te3ⁱⁱ	87.028 (9)	Zr2^iv—Te4—CU7	135.930 (5)
Te3ⁱ—Zr2—Te3ⁱⁱⁱ	96.691 (9)	Zr2^v—Te4—CU5^x	126.340 (11)
Te3ⁱ—Zr2—Te4	86.881 (10)	Zr2^v—Te4—CU5^xi	69.692 (5)
Te3ⁱ—Zr2—Te4^iv	94.416 (9)	Zr2^v—Te4—CU7	135.930 (5)
Te3ⁱ—Zr2—Te4^v	174.6393 (11)	CU5^x—Te4—CU5^xi	89.543 (9)
Te3ⁱⁱ—Zr2—Te3ⁱⁱⁱ	96.691 (9)	CU5^x—Te4—CU7	91.352 (10)
Te3ⁱⁱ—Zr2—Te4	86.881 (10)	CU5^xi—Te4—CU7	91.352 (10)
Te3ⁱⁱ—Zr2—Te4^iv	174.6393 (11)	Te3ⁱⁱⁱ—CU5—Te3^xii	180.0
Te3ⁱⁱ—Zr2—Te4^v	94.416 (9)	Te3ⁱⁱⁱ—CU5—Te4^xiii	89.068 (10)
Te3ⁱⁱⁱ—Zr2—Te4	175.0574 (12)	Te3ⁱⁱⁱ—CU5—Te4^xiv	89.068 (10)
Te3ⁱⁱⁱ—Zr2—Te4^iv	88.276 (10)	Te3ⁱⁱⁱ—CU5—Te4^iv	90.932 (10)
Te3ⁱⁱⁱ—Zr2—Te4^v	88.276 (10)	Te3ⁱⁱⁱ—CU5—Te4^v	90.932 (10)
Te4—Zr2—Te4^iv	88.042 (10)	Te3^xii—CU5—Te4^xiii	90.932 (10)
Te4—Zr2—Te4^v	88.042 (10)	Te3^xii—CU5—Te4^xiv	90.932 (10)
Te4^iv—Zr2—Te4^v	83.686 (9)	Te3^xii—CU5—Te4^iv	89.068 (10)
Zr2ⁱⁱ—Te3—Zr2^vi	87.028 (9)	Te3^xii—CU5—Te4^v	89.068 (10)
Zr2ⁱⁱ—Te3—Zr2^vii	83.309 (9)	Te4^xiii—CU5—Te4^xiv	89.543 (9)
Zr2ⁱⁱ—Te3—CU5^vii	132.375 (5)	Te4^xiii—CU5—Te4^iv	90.457 (9)
Zr2ⁱⁱ—Te3—CU7^viii	71.640 (5)	Te4^xiii—CU5—Te4^v	180.0
Zr2ⁱⁱ—Te3—CU7^ix	130.352 (10)	Te4^xiv—CU5—Te4^iv	180.0
Zr2^vi—Te3—Zr2^vii	83.309 (9)	Te4^xiv—CU5—Te4^v	90.457 (9)
Zr2^vi—Te3—CU5^vii	132.375 (5)	Te4^iv—CU5—Te4^v	89.543 (9)
Zr2^vi—Te3—CU7^viii	130.352 (10)	Te3^xv—CU7—Te3^xvi	88.681 (10)
Zr2^vi—Te3—CU7^ix	71.640 (5)	Te3^xv—CU7—Te3ⁱ	91.319 (10)
Zr2^vii—Te3—CU5^vii	77.580 (13)	Te3^xv—CU7—Te3ⁱⁱ	180.0
Zr2^vii—Te3—CU7^viii	134.869 (5)	Te3^xv—CU7—Te4	87.453 (10)
Zr2^vii—Te3—CU7^ix	134.869 (5)	Te3^xv—CU7—Te4^xvii	92.547 (10)
CU5^vii—Te3—CU7^viii	92.124 (10)	Te3^xvi—CU7—Te3ⁱ	180.0
CU5^vii—Te3—CU7^ix	92.124 (10)	Te3^xvi—CU7—Te3ⁱⁱ	91.319 (10)
CU7^viii—Te3—CU7^ix	88.681 (10)	Te3^xvi—CU7—Te4	87.453 (10)
Zr2—Te4—Zr2^iv	91.958 (10)	Te3^xvi—CU7—Te4^xvii	92.547 (10)
Zr2—Te4—Zr2^v	91.958 (10)	Te3ⁱ—CU7—Te3ⁱⁱ	88.681 (10)
Zr2—Te4—CU5^x	133.020 (5)	Te3ⁱ—CU7—Te4	92.547 (10)
Zr2—Te4—CU5^xi	133.020 (5)	Te3ⁱ—CU7—Te4^xvii	87.453 (10)
Zr2—Te4—CU7	72.046 (13)	Te3ⁱⁱ—CU7—Te4	92.547 (10)
Zr2^iv—Te4—Zr2^v	83.686 (9)	Te3ⁱⁱ—CU7—Te4^xvii	87.453 (10)
Zr2^iv—Te4—CU5^x	69.692 (5)	Te4—CU7—Te4^xvii	180.0
Zr2^iv—Te4—CU5^xi	126.340 (11)

Symmetry codes: (i) −x, y−1, −z+1; (ii) −x, y, −z+1; (iii) x−1/2, y−1/2, z−1/2; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) −x, y+1, −z+1; (vii) x+1/2, y+1/2, z+1/2; (viii) x, y, z+1; (ix) x, y+1, z+1; (x) x+1/2, y−1/2, z−1/2; (xi) x+1/2, y+1/2, z−1/2; (xii) −x+1/2, y−1/2, −z+3/2; (xiii) x−1/2, y−1/2, z+1/2; (xiv) x−1/2, y+1/2, z+1/2; (xv) x, y−1, z−1; (xvi) x, y, z−1; (xvii) −x, y, −z.

(SINCU05ZRTE2_phase_2) top

Crystal data top

Cu	a = 3.594 (3) Å
M_r = 63.55	V = 46.43 (12) Å³
Cubic, Fm3m	Z = 4

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
CU1	0.0	0.0	0.0	0.025*

Geometric parameters (Å, º) top

CU1—CU1ⁱ	2.5415 (16)	CU1—CU1^vii	2.5415 (16)
CU1—CU1ⁱⁱ	2.5415 (16)	CU1—CU1^viii	2.5415 (16)
CU1—CU1ⁱⁱⁱ	2.5415 (16)	CU1—CU1^ix	2.542 (2)
CU1—CU1^iv	2.5415 (16)	CU1—CU1^x	2.542 (2)
CU1—CU1^v	2.5415 (16)	CU1—CU1^xi	2.542 (2)
CU1—CU1^vi	2.5415 (16)	CU1—CU1^xii	2.542 (2)

CU1ⁱ—CU1—CU1ⁱⁱ	90.00 (7)	CU1^iv—CU1—CU1^viii	60.00 (4)
CU1ⁱ—CU1—CU1ⁱⁱⁱ	90.00 (7)	CU1^iv—CU1—CU1^ix	120.00 (2)
CU1ⁱ—CU1—CU1^iv	180.0	CU1^iv—CU1—CU1^x	60.00 (2)
CU1ⁱ—CU1—CU1^v	60.00 (4)	CU1^iv—CU1—CU1^xi	120.00 (2)
CU1ⁱ—CU1—CU1^vi	120.00 (4)	CU1^iv—CU1—CU1^xii	60.00 (2)
CU1ⁱ—CU1—CU1^vii	60.00 (4)	CU1^v—CU1—CU1^vi	90.00 (7)
CU1ⁱ—CU1—CU1^viii	120.00 (4)	CU1^v—CU1—CU1^vii	90.00 (7)
CU1ⁱ—CU1—CU1^ix	60.00 (2)	CU1^v—CU1—CU1^viii	180.0
CU1ⁱ—CU1—CU1^x	120.00 (2)	CU1^v—CU1—CU1^ix	60.00 (2)
CU1ⁱ—CU1—CU1^xi	60.00 (2)	CU1^v—CU1—CU1^x	60.00 (2)
CU1ⁱ—CU1—CU1^xii	120.00 (2)	CU1^v—CU1—CU1^xi	120.00 (2)
CU1ⁱⁱ—CU1—CU1ⁱⁱⁱ	180.0	CU1^v—CU1—CU1^xii	120.00 (2)
CU1ⁱⁱ—CU1—CU1^iv	90.00 (7)	CU1^vi—CU1—CU1^vii	180.0
CU1ⁱⁱ—CU1—CU1^v	120.00 (4)	CU1^vi—CU1—CU1^viii	90.00 (7)
CU1ⁱⁱ—CU1—CU1^vi	60.00 (4)	CU1^vi—CU1—CU1^ix	60.00 (2)
CU1ⁱⁱ—CU1—CU1^vii	120.00 (4)	CU1^vi—CU1—CU1^x	60.00 (2)
CU1ⁱⁱ—CU1—CU1^viii	60.00 (4)	CU1^vi—CU1—CU1^xi	120.00 (2)
CU1ⁱⁱ—CU1—CU1^ix	60.00 (2)	CU1^vi—CU1—CU1^xii	120.00 (2)
CU1ⁱⁱ—CU1—CU1^x	120.00 (2)	CU1^vii—CU1—CU1^viii	90.00 (7)
CU1ⁱⁱ—CU1—CU1^xi	60.00 (2)	CU1^vii—CU1—CU1^ix	120.00 (2)
CU1ⁱⁱ—CU1—CU1^xii	120.00 (2)	CU1^vii—CU1—CU1^x	120.00 (2)
CU1ⁱⁱⁱ—CU1—CU1^iv	90.00 (7)	CU1^vii—CU1—CU1^xi	60.00 (2)
CU1ⁱⁱⁱ—CU1—CU1^v	60.00 (4)	CU1^vii—CU1—CU1^xii	60.00 (2)
CU1ⁱⁱⁱ—CU1—CU1^vi	120.00 (4)	CU1^viii—CU1—CU1^ix	120.00 (2)
CU1ⁱⁱⁱ—CU1—CU1^vii	60.00 (4)	CU1^viii—CU1—CU1^x	120.00 (2)
CU1ⁱⁱⁱ—CU1—CU1^viii	120.00 (4)	CU1^viii—CU1—CU1^xi	60.00 (2)
CU1ⁱⁱⁱ—CU1—CU1^ix	120.00 (2)	CU1^viii—CU1—CU1^xii	60.00 (2)
CU1ⁱⁱⁱ—CU1—CU1^x	60.00 (2)	CU1^ix—CU1—CU1^x	90.0
CU1ⁱⁱⁱ—CU1—CU1^xi	120.00 (2)	CU1^ix—CU1—CU1^xi	90.0
CU1ⁱⁱⁱ—CU1—CU1^xii	60.00 (2)	CU1^ix—CU1—CU1^xii	180.0
CU1^iv—CU1—CU1^v	120.00 (4)	CU1^x—CU1—CU1^xi	180.0
CU1^iv—CU1—CU1^vi	60.00 (4)	CU1^x—CU1—CU1^xii	90.0
CU1^iv—CU1—CU1^vii	120.00 (4)	CU1^xi—CU1—CU1^xii	90.0

Symmetry codes: (i) x, y−1/2, z−1/2; (ii) x, y−1/2, z+1/2; (iii) x, y+1/2, z−1/2; (iv) x, y+1/2, z+1/2; (v) x−1/2, y, z−1/2; (vi) x−1/2, y, z+1/2; (vii) x+1/2, y, z−1/2; (viii) x+1/2, y, z+1/2; (ix) x−1/2, y−1/2, z; (x) x−1/2, y+1/2, z; (xi) x+1/2, y−1/2, z; (xii) x+1/2, y+1/2, z.

(SINCU05ZRTE2_phase_3) top

Crystal data top

Te₂Zr	c = 6.7455 (18) Å
M_r = 346.42	V = 91.85 (3) Å³
Trigonal, P3m1	Z = 1
a = 3.9652 (6) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
ZR1	0.0	0.0	0.0	0.4412
TE2	0.33333	0.66667	0.25972	0.47166

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
ZR1	0.43123	0.43123	0.46113	0.21562	0.0	0.0
TE2	0.15541	0.15541	0.63083	−0.2773	0.0	0.0

Geometric parameters (Å, º) top

ZR1—TE2ⁱ	2.8827 (4)	ZR1—TE2^v	2.8827 (4)
ZR1—TE2ⁱⁱ	2.8827 (4)	TE2—ZR1	2.8827 (4)
ZR1—TE2	2.8827 (4)	TE2—ZR1^vi	2.8827 (4)
ZR1—TE2ⁱⁱⁱ	2.8827 (4)	TE2—ZR1^vii	2.8827 (4)
ZR1—TE2^iv	2.8827 (4)

TE2ⁱ—ZR1—TE2ⁱⁱ	86.904 (12)	TE2—ZR1—TE2ⁱⁱⁱ	180.0
TE2ⁱ—ZR1—TE2	86.904 (12)	TE2—ZR1—TE2^iv	93.096 (12)
TE2ⁱ—ZR1—TE2ⁱⁱⁱ	93.096 (12)	TE2—ZR1—TE2^v	93.096 (12)
TE2ⁱ—ZR1—TE2^iv	93.096 (12)	TE2ⁱⁱⁱ—ZR1—TE2^iv	86.904 (12)
TE2ⁱ—ZR1—TE2^v	180.0	TE2ⁱⁱⁱ—ZR1—TE2^v	86.904 (12)
TE2ⁱⁱ—ZR1—TE2	86.904 (12)	TE2^iv—ZR1—TE2^v	86.904 (12)
TE2ⁱⁱ—ZR1—TE2ⁱⁱⁱ	93.096 (12)	ZR1—TE2—ZR1^vi	86.904 (12)
TE2ⁱⁱ—ZR1—TE2^iv	180.0	ZR1—TE2—ZR1^vii	86.904 (12)
TE2ⁱⁱ—ZR1—TE2^v	93.096 (12)	ZR1^vi—TE2—ZR1^vii	86.904 (12)

Symmetry codes: (i) x−1, y−1, z; (ii) x, y−1, z; (iii) −x, −y, −z; (iv) −x, −y+1, −z; (v) −x+1, −y+1, −z; (vi) x, y+1, z; (vii) x+1, y+1, z.

(SINCU05ZRTE2_phase_4) top

Crystal data top

Te₃Zr	c = 10.086 (2) Å
M_r = 474.02	β = 96.32 (5)°
Monoclinic, P2₁/m	V = 236.85 (17) Å³
a = 6.176 (4) Å	Z = 2
b = 3.825 (2) Å

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
CU1	0.95236	0.25	0.68273	0.025*
CU2	−0.11809	0.25	0.49533	0.025*
TE3	0.31131	0.25	0.16968	0.025*
TE4	−0.09227	0.25	0.10972	0.025*

Geometric parameters (Å, º) top

CU1—CU2ⁱ	1.8924 (5)	TE3—CU1ⁱⁱ	3.0100 (12)
CU1—CU2ⁱⁱ	2.8873 (10)	TE3—CU1ⁱⁱⁱ	3.0100 (12)
CU1—CU2ⁱⁱⁱ	2.8873 (10)	TE3—TE4	2.4993 (15)
CU1—TE3ⁱⁱ	3.0100 (12)	TE3—TE4^vii	3.5483 (12)
CU1—TE3ⁱⁱⁱ	3.0100 (12)	TE3—TE4^viii	3.5483 (12)
CU1—TE4ⁱⁱ	2.8964 (10)	TE4—CU1ⁱⁱ	2.8964 (10)
CU1—TE4ⁱⁱⁱ	2.8964 (10)	TE4—CU1ⁱⁱⁱ	2.8964 (10)
CU2—CU1^iv	1.8924 (5)	TE4—TE3	2.4993 (15)
CU2—CU1ⁱⁱ	2.8873 (10)	TE4—TE3^vii	3.5483 (12)
CU2—CU1ⁱⁱⁱ	2.8873 (10)	TE4—TE3^viii	3.5483 (12)
CU2—CU2^v	2.4010 (11)	TE4—TE4^vii	3.2267 (11)
CU2—CU2^vi	2.4010 (11)	TE4—TE4^viii	3.2267 (11)

CU2ⁱ—CU1—CU2ⁱⁱ	55.73 (2)	TE3ⁱⁱⁱ—CU1—TE4ⁱⁱⁱ	50.02 (3)
CU2ⁱ—CU1—CU2ⁱⁱⁱ	55.73 (2)	TE4ⁱⁱ—CU1—TE4ⁱⁱⁱ	82.66 (4)
CU2ⁱ—CU1—TE3ⁱⁱ	114.62 (3)	CU1^iv—CU2—CU1ⁱⁱ	124.27 (2)
CU2ⁱ—CU1—TE3ⁱⁱⁱ	114.62 (3)	CU1^iv—CU2—CU1ⁱⁱⁱ	124.27 (2)
CU2ⁱ—CU1—TE4ⁱⁱ	137.68 (2)	CU1^iv—CU2—CU2^v	83.62 (3)
CU2ⁱ—CU1—TE4ⁱⁱⁱ	137.68 (2)	CU1^iv—CU2—CU2^vi	83.62 (3)
CU2ⁱⁱ—CU1—CU2ⁱⁱⁱ	82.97 (4)	CU1ⁱⁱ—CU2—CU1ⁱⁱⁱ	82.97 (4)
CU2ⁱⁱ—CU1—TE3ⁱⁱ	97.75 (4)	CU1ⁱⁱ—CU2—CU2^v	40.64 (2)
CU2ⁱⁱ—CU1—TE3ⁱⁱⁱ	167.616 (9)	CU1ⁱⁱ—CU2—CU2^vi	107.26 (4)
CU2ⁱⁱ—CU1—TE4ⁱⁱ	85.07 (3)	CU1ⁱⁱⁱ—CU2—CU2^v	107.26 (4)
CU2ⁱⁱ—CU1—TE4ⁱⁱⁱ	142.10 (2)	CU1ⁱⁱⁱ—CU2—CU2^vi	40.64 (2)
CU2ⁱⁱⁱ—CU1—TE3ⁱⁱ	167.616 (9)	CU2^v—CU2—CU2^vi	105.62 (5)
CU2ⁱⁱⁱ—CU1—TE3ⁱⁱⁱ	97.75 (4)	CU1ⁱⁱ—TE3—CU1ⁱⁱⁱ	78.91 (5)
CU2ⁱⁱⁱ—CU1—TE4ⁱⁱ	142.10 (2)	CU1ⁱⁱ—TE3—TE4	62.63 (3)
CU2ⁱⁱⁱ—CU1—TE4ⁱⁱⁱ	85.07 (3)	CU1ⁱⁱⁱ—TE3—TE4	62.63 (3)
TE3ⁱⁱ—CU1—TE3ⁱⁱⁱ	78.91 (5)	CU1ⁱⁱ—TE4—CU1ⁱⁱⁱ	82.66 (4)
TE3ⁱⁱ—CU1—TE4ⁱⁱ	50.02 (3)	CU1ⁱⁱ—TE4—TE3	67.35 (3)
TE3ⁱⁱ—CU1—TE4ⁱⁱⁱ	101.35 (3)	CU1ⁱⁱⁱ—TE4—TE3	67.35 (3)
TE3ⁱⁱⁱ—CU1—TE4ⁱⁱ	101.35 (3)

Symmetry codes: (i) x+1, y, z; (ii) −x+1, y−1/2, −z+1; (iii) −x+1, y+1/2, −z+1; (iv) x−1, y, z; (v) −x, y−1/2, −z+1; (vi) −x, y+1/2, −z+1; (vii) −x, y−1/2, −z; (viii) −x, y+1/2, −z.

The results of the crystal structure refinement of Cu_0.5ZrTe₂ at room temperature. Cu atoms, which occupy octahedral sites, are designated as Cu^O. The CIF file containing all the phases is available in the supporting information. top

Cu_xZrTe₂, weight fraction 62.5 (6)%
I/2m; a = 6.832 (1), b = 3.9517 (2) and c = 13.2455 (5) Å, and β = 89.97 (1)°
Atom type	x	y	z	Mult.	Occupation
Zr	-0.025 (3)	0	0.251 (1)	4	1
Te	0.187 (1)	1/2	0.8817 (3)	4	1
Te	0.322 (1)	0	0.1192 (2)	4	1
Cu^O	0	0	1/2	2	1.00 (2)
Cu^O	0	0	0	2	0.24 (2)
ZrTe₂, weight fraction 31.9 (8)%
ZrTe₃, weight fraction 3.8 (2)%
Cu, weight fraction 1.8 (2)%
R_F² = 6.26%, wR_p = 8.60%, R_p = 6.48%, χ² = 7.246

The results of the crystal structure refinement for Cu_0.5ZrTe₂ at 500°C. Cu atoms, which occupy tetrahedral sites, are designated as Cu^T. The CIF file containing all the phases is available in the supporting information. top

Cu_xZrTe₂, weight fraction 31.0 (4)%
I/2m; a = 6.8971 (7), b = 3.9764 (3) and c = 13.3966 (4) Â, and β = 90.130 (7)°
Atom type	x	y	z	Mult.	Occupation
Zr	0.018 (3)	0	0.249 (1)	4	1
Te	0.147 (2)	1/2	0.8834 (4)	4	1.00 (1)
Te	0.332 (2)	0	0.1224 (4)	4	1.00 (1)
Cu^T	0.226 (7)	1/2	0.038 (2)	4	0.54 (1)
Zr	0	0	1/2	2	0.09 (1)
ZrTe_1,6, weight fraction 15.7 (5)%
ZrTe₃, weight fraction 21.3 (4)%
Cu₇Te₄, weight fraction 5.4 (3)%
CuZr₂Te₄, weight fraction 26.7 (7)%
R3m; a = 7.096 (2) and c = 39.43 (1) Å
Atom type	x	y	z	Mult.	Occupation
Cu	0	0	0.133 (1)	6	1
Cu	0	0	0.342 (1)	6	1
Zr	0	0	0	3	1
Zr	0.225 (5)	0.113 (3)	0.1106 (4)	18	1
Zr	0	0	1/2	3	1
Te	0	0	0.1787 (6)	6	1
Te	0	0	0.283 (2)	6	1
Te	0.22 (1)	0.44 (1)	0.405 (1)	18	1
Te	0.134 (4)	0.268 (7)	0.030 (1)	18	1
R(F²) = 7.96%, wR_p = 8.14%, R_p = 6.11%, χ² = 10.16

The results of the crystal structure refinement of the Cu_0.5ZrTe₂ after annealing at 467°C for one week. Cu atoms, which occupy tetrahedral sites, are designated as Cu^T. The CIF file containing all the phases is available in the supporting information. top

Cu_xZrTe₂, weight fraction 64.1 (3)%
I/2m; a = 6.8572 (7), b = 3.9470 (7) and c = 13.250 (1) Å, and β = 90.18 (1)°
Atom type	x	y	z	Mult.	Occupation
Zr	0.005 (3)	0	0.248 (2)	4	0.99 (1)
Te	0.162 (1)	1/2	0.890 (1)	4	0.99 (1)
Te	0.325 (1)	0	0.119 (1)	4	0.98 (1)
Cu^T	0.18 (9)	1/2	-0.03 (3)	4	0.04 (2)
Zr	0	0	1/2	2	0.21 (3)
ZrTe₃, weight fraction 16.8 (4)%
Cu₇Te₄, weight fraction 14.9 (4)%
CuZr₂Te₄, weight fraction 4.2 (2)%
R3m; a = 7.051 (5) and c = 39.45 (1) Å
Atom type	x	y	z	Mult.	Occupation
Cu	0	0	0.145 (2)	6	0.9 (2)
Cu	0	0	-0.387 (2)	6	1
Zr	0	0	0	3	1
Zr	0.03 (2)	0.0 (1)	0.081 (1)	18	1
Zr	0	0	1/2	3	1
Te	0	0	0.149 (1)	6	0.91 (8)
Te	0	0	0.326 (1)	6	1
Te	0.427 (6)	0.85 (1)	0.401 (1)	18	0.90 (3)
Te	0.115 (5)	0.22 (1)	0.202 (1)	18	1.00 (4)
R(F²) = 8.23%, wR_p = 17.05%, R_p = 12.26%, χ² = 6.593

The results of the crystal structure refinement for Cu_0.5ZrTe₂ at 900°C. Cu atoms, which occupy octahedral voids, are designated as Cu^O. Cu atoms, which occupy tetrahedral sites, are designated as Cu^T. The CIF file containing all the phases is available in the supporting information. top

Cu_xZrTe₂, weight fraction 37.9 (6)% I/2m; a = 9495 (5), b = 4.0169 (2) and c = 13.5472 (3) Å, and β = 90.900 (5)°
Atom type	x	y	z	Mult.	Occupation
Zr	0.001 (3)	0	0.250 (1)	4	1
Te	0.164 (3)	1/2	0.8766 (4)	4	1.00 (1)
Te	0.342 (2)	0	0.1192 (4)	4	1.00 (1)
Cu^O	0	0	1/2	2	0.23 (3)
Cu^O	1/2	0	0	2	0.40 (2)
Cu^T	0.327 (4)	1/2	0.153 (2)	4	0.69 (2)
Cu^T	0.788 (6)	1/2	0.427 (1)	4	0.37 (1)
Zr	0	0	0	2	0.07 (1)
ZrTe₂, weight fraction 17.1 (3)%
ZrTe₃, weight fraction 39.9 (7)%
SiO₂, weight fraction 5.0 (3)%
R(F²) = 8.36%, wR_p = 6.34%, R_p = 4.81%, χ² = 6.473

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
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Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

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