Crystal structure variations in the series SrLnCuS3 (Ln = La, Pr, Sm, Gd, Er and Lu)

Ruseikina, A.V.; Solovyov, L.A.; Grigoriev, M.V.; Andreev, O.V.

doi:10.1107/S2053229619004984

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Crystal structure variations in the series SrLnCuS₃ (Ln = La, Pr, Sm, Gd, Er and Lu)

A. V. Ruseikina, L. A. Solovyov, M. V. Grigoriev and O. V. Andreev

The crystal structures of the complex sulfides SrLnCuS₃ (Ln = Sm, Gd, Er and Lu) have been determined and refined using powder X-ray diffraction. The crystals are found to be orthorhombic, with the structure type changing consecutively in the order BaLaCuS₃ → Eu₂CuS₃ → KZrCuS₃ as the Ln³⁺ ionic radius decreases in the order La/Pr → Sm/Gd → Er/Lu. Variations of the structure parameters along the series of compounds studied are analyzed, and an effect caused by crystallochemical contraction on the stabilization of the respective structure types is demonstrated.

Keywords: powder diffraction; crystallochemical contraction; sulfides of rare earth elements; SrLnCuS₃; derivative difference minimization method; powder diffraction; crystal structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229619004984/lg3238sup1.cif Contains datablocks global, SrErCuS3, SrGdCuS3, SrLuCuS3, SrSmCuS3
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S2053229619004984/lg3238SrErCuS3sup2.rtv Contains datablock SrErCuS3
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S2053229619004984/lg3238SrGdCuS3sup3.rtv Contains datablock SrGdCuS3
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S2053229619004984/lg3238SrLuCuS3sup4.rtv Contains datablock SrLuCuS3
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S2053229619004984/lg3238SrSmCuS3sup5.rtv Contains datablock SrSmCuS3

CCDC references: 1909592; 1909591; 1909590; 1909589

Computing details top

For all structures, program(s) used to refine structure: Powder diffraction, Derivative Difference Method (DDM) (Solovyov, 2004).

Strontium erbium copper trisulfide (SrErCuS3) top

Crystal data top

SrErCuS₃	V = 513.99 (1) Å³
M_r = 414.54	Z = 4
Orthorhombic, Cmcm	D_x = 5.359 Mg m⁻³
Hall symbol: -C 2C 2	Cu Kα radiation
a = 3.92672 (5) Å	T = 298 K
b = 12.9632 (2) Å	yellow
c = 10.0974 (1) Å

Data collection top

PANalytical X'Pert PRO
diffractometer

2θ_min = 10.007°, 2θ_max = 139.996°, 2θ_step = 0.013°

Refinement top

Least-squares matrix: full	R(F) = 0.026
R_wp = 0.057	22 parameters
R_exp = 0.016	0 restraints
R_Bragg = 0.031	(Δ/σ)_max = 0.004

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

	x	y	z	U_iso*/U_eq
Er	0.00000	0.00000	0.00000	0.0118 (10)
Sr	0.00000	0.74764 (12)	0.25000	0.0176 (11)
Cu	0.00000	0.47116 (17)	0.25000	0.0176 (12)
S1	0.00000	0.3642 (2)	0.0658 (3)	0.0169 (12)
S2	0.00000	0.0755 (3)	0.25000	0.0114 (14)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Er	0.0066 (11)	0.0122 (11)	0.0167 (12)	0.0000	0.0000	0.0010 (6)
Sr	0.0127 (14)	0.0138 (13)	0.0265 (15)	0.0000	0.0000	0.0000
Cu	0.022 (2)	0.0153 (18)	0.0155 (18)	0.0000	0.0000	0.0000
S1	0.023 (2)	0.0055 (19)	0.023 (2)	0.0000	0.0000	−0.0028 (16)
S2	0.013 (3)	0.010 (3)	0.012 (2)	0.0000	0.0000	0.0000

Geometric parameters (Å, º) top

Er—S1ⁱ	2.7194 (19)	Sr—S2ⁱⁱ	2.972 (3)
Er—S2	2.7074 (13)	Cu—S1	2.320 (3)
Sr—S1ⁱⁱ	3.098 (2)	Cu—S2ⁱⁱ	2.384 (2)

S1ⁱ—Er—S1ⁱⁱⁱ	92.44 (8)	S1ⁱⁱ—Sr—S2ⁱⁱ	86.99 (5)
S1ⁱ—Er—S1^iv	87.56 (8)	S1ⁱⁱ—Sr—S2^vi	141.70 (6)
S1ⁱ—Er—S2	90.36 (8)	S2ⁱⁱ—Sr—S2^vi	82.68 (10)
S1ⁱ—Er—S2^v	89.64 (8)	S1—Cu—S1^ix	106.59 (16)
S1ⁱⁱ—Sr—S1^vi	78.65 (7)	S1—Cu—S2ⁱⁱ	109.82 (5)
S1ⁱⁱ—Sr—S1^vii	73.80 (10)	S2ⁱⁱ—Cu—S2^vi	110.87 (16)
S1ⁱⁱ—Sr—S1^viii	121.62 (11)

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

Strontium gadolinium copper trisulfide (SrGdCuS3) top

Crystal data top

SrGdCuS₃	V = 529.62 (2) Å³
M_r = 404.54	Z = 4
Orthorhombic, Pnma	D_x = 5.075 Mg m⁻³
Hall symbol: -P 2AC 2N	Cu Kα radiation
a = 10.3288 (2) Å	T = 298 K
b = 3.96271 (7) Å	yellow
c = 12.9397 (2) Å

Data collection top

PANalytical X'Pert PRO
diffractometer

2θ_min = 10.007°, 2θ_max = 139.996°, 2θ_step = 0.013°

Refinement top

Least-squares matrix: full	R(F) = 0.022
R_wp = 0.044	36 parameters
R_exp = 0.016	0 restraints
R_Bragg = 0.025	(Δ/σ)_max = 0.021

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

	x	y	z	U_iso*/U_eq
Gd	0.01504 (11)	0.25000	0.74014 (7)	0.0111 (9)
Sr	0.77629 (16)	0.25000	0.00231 (11)	0.0141 (10)
Cu	0.2346 (2)	0.25000	0.22237 (17)	0.0193 (12)
S1	0.0521 (4)	0.25000	0.1178 (2)	0.0101 (15)
S2	0.4085 (4)	0.25000	0.1067 (3)	0.0077 (15)
S3	0.2612 (4)	0.25000	0.8273 (3)	0.0099 (14)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd	0.0104 (13)	0.0092 (12)	0.0139 (11)	0.0000	0.0003 (6)	0.0000
Sr	0.0221 (18)	0.0099 (14)	0.0102 (13)	0.0000	−0.0005 (10)	0.0000
Cu	0.014 (2)	0.019 (2)	0.026 (2)	0.0000	−0.0017 (15)	0.0000
S1	0.012 (3)	0.017 (6)	0.002 (3)	0.0000	−0.001 (2)	0.0000
S2	0.014 (3)	0.005 (5)	0.004 (3)	0.0000	−0.001 (2)	0.0000
S3	0.012 (3)	0.004 (3)	0.015 (3)	0.0000	−0.003 (3)	0.0000

Geometric parameters (Å, º) top

Gd—S1ⁱ	2.791 (2)	Sr—S2^v	3.092 (3)
Gd—S2ⁱⁱ	2.745 (3)	Sr—S3^vi	2.990 (3)
Gd—S3	2.781 (4)	Cu—S1	2.320 (4)
Gd—S3ⁱⁱⁱ	2.763 (4)	Cu—S2	2.339 (5)
Sr—S1^iv	3.217 (4)	Cu—S3^vii	2.402 (2)
Sr—S1^v	3.079 (3)

S1ⁱ—Gd—S1^viii	90.47 (9)	S1^v—Sr—S2^v	73.32 (9)
S1ⁱ—Gd—S2ⁱⁱ	88.49 (7)	S1^v—Sr—S2^x	122.53 (9)
S1ⁱ—Gd—S2^ix	177.11 (12)	S1^v—Sr—S3^vi	91.16 (7)
S1ⁱ—Gd—S3	87.72 (10)	S1^v—Sr—S3^xi	150.83 (12)
S1ⁱ—Gd—S3ⁱⁱⁱ	88.40 (10)	S2^v—Sr—S2^x	79.72 (10)
S2ⁱⁱ—Gd—S2^ix	92.42 (11)	S2^v—Sr—S3^vi	80.31 (8)
S2ⁱⁱ—Gd—S3	89.55 (10)	S2^v—Sr—S3^xi	132.93 (12)
S2ⁱⁱ—Gd—S3ⁱⁱⁱ	94.26 (10)	S3^vi—Sr—S3^xi	83.01 (9)
S3—Gd—S3ⁱⁱⁱ	174.49 (7)	S1—Cu—S2	104.50 (15)
S1^iv—Sr—S1^v	74.01 (8)	S1—Cu—S3^vii	110.14 (12)
S1^iv—Sr—S2^v	139.34 (6)	S2—Cu—S3^vii	110.35 (12)
S1^iv—Sr—S3^vi	76.83 (9)	S3^vii—Cu—S3^xii	111.15 (16)
S1^v—Sr—S1^x	80.10 (9)

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

Strontium lutetium copper trisulfide (SrLuCuS3) top

Crystal data top

SrLuCuS₃	V = 507.54 (1) Å³
M_r = 422.31	Z = 4
Orthorhombic, Cmcm	D_x = 5.529 Mg m⁻³
Hall symbol: -C 2C 2	Cu Kα radiation
a = 3.91105 (4) Å	T = 298 K
b = 12.9504 (1) Å	purple
c = 10.0206 (1) Å

Data collection top

PANalytical X'Pert PRO
diffractometer

2θ_min = 10.007°, 2θ_max = 139.996°, 2θ_step = 0.013°

Refinement top

Least-squares matrix: full	R(F) = 0.013
R_wp = 0.053	22 parameters
R_exp = 0.015	0 restraints
R_Bragg = 0.027	(Δ/σ)_max = 0.010

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

	x	y	z	U_iso*/U_eq
Lu	0.00000	0.00000	0.00000	0.0081 (8)
Sr	0.00000	0.74784 (9)	0.25000	0.0097 (8)
Cu	0.00000	0.47066 (13)	0.25000	0.0097 (9)
S1	0.00000	0.36458 (17)	0.0637 (4)	0.0064 (8)
S2	0.00000	0.0758 (3)	0.25000	0.0059 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Lu	0.0062 (10)	0.0096 (8)	0.0086 (11)	0.0000	0.0000	−0.0010 (4)
Sr	0.0033 (10)	0.0073 (10)	0.0183 (16)	0.0000	0.0000	0.0000
Cu	0.0154 (15)	0.0091 (13)	0.0048 (17)	0.0000	0.0000	0.0000
S1	0.0045 (15)	0.0072 (13)	0.0074 (12)	0.0000	0.0000	−0.0029 (11)
S2	0.007 (2)	0.0052 (19)	0.006 (2)	0.0000	0.0000	0.0000

Geometric parameters (Å, º) top

Lu—S1ⁱ	2.7030 (17)	Sr—S2ⁱⁱ	2.965 (3)
Lu—S2	2.6905 (13)	Cu—S1	2.318 (3)
Sr—S1ⁱⁱ	3.098 (3)	Cu—S2ⁱⁱ	2.383 (2)

S1ⁱ—Lu—S1ⁱⁱⁱ	92.68 (7)	S1ⁱⁱ—Sr—S2ⁱⁱ	87.16 (5)
S1ⁱ—Lu—S1^iv	87.32 (7)	S1ⁱⁱ—Sr—S2^vi	141.55 (6)
S1ⁱ—Lu—S2	90.97 (9)	S2ⁱⁱ—Sr—S2^vi	82.54 (10)
S1ⁱ—Lu—S2^v	89.03 (9)	S1—Cu—S1^ix	107.31 (15)
S1ⁱⁱ—Sr—S1^vi	78.29 (7)	S1—Cu—S2ⁱⁱ	109.79 (5)
S1ⁱⁱ—Sr—S1^vii	74.14 (11)	S2ⁱⁱ—Cu—S2^vi	110.32 (16)
S1ⁱⁱ—Sr—S1^viii	121.57 (9)

Strontium samarium copper trisulfide (SrSmCuS3) top

Crystal data top

SrSmCuS₃	V = 537.63 (2) Å³
M_r = 397.74	Z = 4
Orthorhombic, Pnma	D_x = 4.916 Mg m⁻³
Hall symbol: -P 2AC 2N	Cu Kα radiation
a = 10.4285 (2) Å	T = 298 K
b = 3.98640 (7) Å	yellow
c = 12.9325 (2) Å

Data collection top

PANalytical X'Pert PRO
diffractometer

2θ_min = 10.007°, 2θ_max = 139.996°, 2θ_step = 0.013°

Refinement top

Least-squares matrix: full	R(F) = 0.021
R_wp = 0.049	36 parameters
R_exp = 0.019	0 restraints
R_Bragg = 0.029	(Δ/σ)_max = 0.003

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

	x	y	z	U_iso*/U_eq
Sm	0.01587 (10)	0.25000	0.73736 (7)	0.0093 (12)
Sr	0.78116 (18)	0.25000	0.00217 (11)	0.0089 (12)
Cu	0.2342 (2)	0.25000	0.22281 (18)	0.0159 (14)
S1	0.0504 (4)	0.25000	0.1190 (3)	0.0082 (17)
S2	0.4031 (5)	0.25000	0.1040 (3)	0.0105 (17)
S3	0.2606 (4)	0.25000	0.8264 (3)	0.0096 (17)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sm	0.0096 (16)	0.0081 (16)	0.0102 (13)	0.0000	0.0005 (6)	0.0000
Sr	0.0117 (17)	0.0073 (17)	0.0076 (14)	0.0000	−0.0001 (8)	0.0000
Cu	0.0075 (19)	0.019 (2)	0.021 (2)	0.0000	−0.0014 (16)	0.0000
S1	0.009 (4)	0.005 (5)	0.011 (3)	0.0000	−0.006 (2)	0.0000
S2	0.010 (3)	0.019 (5)	0.003 (3)	0.0000	0.000 (2)	0.0000
S3	0.002 (3)	0.016 (3)	0.012 (3)	0.0000	−0.001 (2)	0.0000

Geometric parameters (Å, º) top

Sm—S1ⁱ	2.811 (3)	Sr—S2^v	3.090 (4)
Sm—S2ⁱⁱ	2.768 (3)	Sr—S3^vi	3.013 (3)
Sm—S3	2.800 (4)	Cu—S1	2.340 (5)
Sm—S3ⁱⁱⁱ	2.787 (5)	Cu—S2	2.337 (5)
Sr—S1^iv	3.188 (5)	Cu—S3^vii	2.402 (2)
Sr—S1^v	3.085 (3)

S1ⁱ—Sm—S1^viii	90.33 (11)	S1^v—Sr—S2^v	73.24 (11)
S1ⁱ—Sm—S2ⁱⁱ	88.63 (8)	S1^v—Sr—S2^x	123.04 (10)
S1ⁱ—Sm—S2^ix	175.91 (13)	S1^v—Sr—S3^vi	91.64 (8)
S1ⁱ—Sm—S3	87.26 (10)	S1^v—Sr—S3^xi	152.08 (13)
S1ⁱ—Sm—S3ⁱⁱⁱ	87.75 (10)	S2^v—Sr—S2^x	80.33 (12)
S2ⁱⁱ—Sm—S2^ix	92.12 (12)	S2^v—Sr—S3^vi	79.07 (9)
S2ⁱⁱ—Sm—S3	88.75 (12)	S2^v—Sr—S3^xi	131.60 (13)
S2ⁱⁱ—Sm—S3ⁱⁱⁱ	96.15 (12)	S3^vi—Sr—S3^xi	82.85 (10)
S3—Sm—S3ⁱⁱⁱ	172.92 (7)	S1—Cu—S2	103.90 (17)
S1^iv—Sr—S1^v	74.89 (10)	S1—Cu—S3^vii	109.79 (13)
S1^iv—Sr—S2^v	139.29 (7)	S2—Cu—S3^vii	110.46 (13)
S1^iv—Sr—S3^vi	77.20 (10)	S3^vii—Cu—S3^xii	112.13 (17)
S1^v—Sr—S1^x	80.50 (10)

Experimental details top

	SrErCuS₃	SrGdCuS₃	SrLuCuS₃	SrSmCuS₃
Crystal data
Chemical formula	CuEr_S3Sr	CuGd_S3Sr	CuLu_S3Sr	Cu_S3SmSr
M_r	414.54	404.54	422.31	397.74
Crystal system, space group	Orthorhombic, Cmcm	Orthorhombic, Pnma	Orthorhombic, Cmcm	Orthorhombic, Pnma
Temperature (K)	298	298	298	298
a, b, c (Å)	3.92672 (5), 12.9632 (2), 10.0974 (1)	10.3288 (2), 3.96271 (7), 12.9397 (2)	3.91105 (4), 12.9504 (1), 10.0206 (1)	10.4285 (2), 3.98640 (7), 12.9325 (2)
V (Å³)	513.99 (1)	529.62 (2)	507.54 (1)	537.63 (2)
Z	4	4	4	4
Radiation type	Cu Kα, λ = 1.5418 Å	Cu Kα, λ = 1.5418 Å	Cu Kα, λ = 1.5418 Å	Cu Kα, λ = 1.5418 Å
Specimen shape, size (mm)	Cylinder, 25 × 25	Cylinder, 25 × 25	Cylinder, 25 × 25	Cylinder, 25 × 25

Data collection
Diffractometer	PANalytical X'Pert PRO	PANalytical X'Pert PRO	PANalytical X'Pert PRO	PANalytical X'Pert PRO
Specimen mounting	Flat plate	Flat plate	Flat plate	Flat plate
Data collection mode	Reflection	Reflection	Reflection	Reflection
Scan method	Step	Step	Step	Step
2θ_min values (°) 2θ_max values (°) 2θ_step values (°)	10.01 140.00 0.013	10.01 140.00 0.013	10.01 140.00 0.013	10.01 140.00 0.013
Time/step (sec)	1.5	1.5	1.5	1.5

Refinement
R_p	0.044	0.037	0.042	0.032
R_wp	0.057	0.044	0.053	0.049
R_exp	0.016	0.016	0.015	0.019
R_Bragg	0.031	0.025	0.027	0.029
R(F)	0.026	0.022	0.013	0.021
χ²	13.155	7.632	11.654	6.627
No. of parameters	22	36	22	36

Computer programs: DDM (Solovyov, 2004)

Interatomic distances (d) and their average values in SrLnCuS₃ structures (Ln = La, Pr, Sm, Gd, Er and Lu) top

Bond	d (Å)	Bond	d (Å)	Bond	d (Å)
SrLCuS₃^a
<La—S>	2.966 (1)^b	<Sr—S>	3.058 (2)^b	<Cu—S>	2.353 (2)^b
	2.96 (5)^c		3.05 (5)^c		2.35 (1)^c

SrPrCuS₃^a
<Pr—S>	2.924 (2)^b	<Sr—S>	3.056 (2)^b	<Cu—S>	2.343 (2)^b
	2.92 (5)^c		3.05 (6)^c		2.34 (2)^c

SrSmCuS₃
Sm—S1	2.811 (3) (×2)	Sr—S1	3.188 (5) (×1)	Cu—S1	2.340 (5) (×1)
Sm—S2	2.768 (3) (×2)	Sr—S1	3.085 (3) (×2)	Cu—S2	2.337 (5) (×1)
Sm—S3	2.800 (4) (×1)	Sr—S2	3.090 (4) (×2)	Cu—S3	2.402 (2) (×2)
Sm—S3	2.787 (5) (×1)	Sr—S3	3.013 (3) (×2)
<Sm—S>	2.792 (2)^b	<Sr—S>	3.080 (2)^b	<Cu—S>	2.372 (2)^b
	2.79 (2)^c		3.08 (6)^c		2.37 (4)^c

SrGdCuS₃
Gd—S1	2.791 (2) (×2)	Sr—S1	3.217 (4) (×1)	Cu—S1	2.320 (4) (×1)
Gd—S2	2.745 (3) (×2)	Sr—S1	3.079 (3) (×2)	Cu—S2	2.339 (5) (×1)
Gd—S3	2.781 (4) (×1)	Sr—S2	3.092 (3) (×2)	Cu—S3	2.402 (2) (×2)
Gd—S3	2.763 (4) (×1)	Sr—S3	2.990 (3) (×2)
<Gd—S>	2.769 (2)^b	<Sr—S>	3.077 (2)^b	<Cu—S>	2.366 (2)^b
	2.77 (2)^c		3.08 (8)^c		2.37 (4)^c

SrErCuS₃
Er—S1	2.719 (2) (×4)	Sr—S1	3.098 (2) (×4)	Cu—S1	2.320 (3) (×2)
Er—S2	2.707 (1) (×2)	Sr—S2	2.972 (3) (×2)	Cu—S2	2.384 (2) (×2)
<Er—S>	2.715 (1)^b	<Sr—S>	3.056 (2)^b	<Cu—S>	2.352 (2)^b
	2.72 (1)^c		3.06 (7)^c		2.35 (4)^c

SrLuCuS₃
Lu—S1	2.703 (2) (×4)	Sr—S1	3.098 (3) (×4)	Cu—S1	2.318 (3) (×2)
Lu—S2	2.691 (1) (×2)	Sr—S2	2.965 (3) (×2)	Cu—S2	2.383 (2) (×2)
<Lu—S>	2.699 (1)^b	<Sr—S>	3.054 (2)^b	<Cu—S>	2.350 (2)^b
	2.699 (6)^c		3.05 (7)^c		2.35 (4)^c

Notes: (a) data for SrLCuS₃ and SrPrCuS₃ are from Ruseikina et al. (2014); (b) experimental error (DDM; Solovyov, 2004); (c) regular variations of distances due to the polyhedron distortion (Bell, 2001).

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