Crystal structure of the ternary silicide Gd2Re3Si5

Fedyna, V.; Kozak, R.; Gladyshevskii, R.

doi:10.1107/S1600536814024234

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Volume 70| Part 12| December 2014| Pages 469-470

doi:10.1107/S1600536814024234

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Crystal structure of the ternary silicide Gd₂Re₃Si₅

Vitaliia Fedyna,^a ^* Roksolana Kozak ^b and Roman Gladyshevskii ^a

^aDepartment of Inorganic Chemistry, Ivan Franko National University of Lviv, Kyryla i Mefodiya st. 6, UA-79005 Lviv, Ukraine, and ^bLaboratory of Crystallography, Department of Materials, ETH Zurich, Vladimir-Prelog-Weg 5, CH-8093 Zurich, Switzerland
^*Correspondence e-mail: vitaliia.fedyna@gmail.com

Edited by L. Farrugia, University of Glasgow, Scotland (Received 20 October 2014; accepted 3 November 2014; online 8 November 2014)

A single crystal of the title compound, the ternary silicide digadolinium trirhenium pentasilicide, Gd₂Re₃Si₅, was isolated from an alloy of nominal composition Gd₂₀Re₃₀Si₅₀ synthesized by arc melting and investigated by X-ray single-crystal diffraction. Its crystal structure belongs to the U₂Mn₃Si₅ structure type. All atoms in the asymmetric lie on special positions. The Gd site has site symmetry m..; the two Mn atoms have site symmetries m.. and 2.22; the three Si atoms have site symmetries m.., ..2 and 4.. . The coordination polyhedra of the Gd atoms have 21 vertices, while those of the Re atoms are cubooctahedra and 13-vertex polyhedra. The Si atoms are arranged as tricapped trigonal prisms, bicapped square antiprisms, or 11-vertex polyhedra. The crystal structure of the title compound is also related to the structure types CaBe₂Ge₂ and W₅Si₃. It can be represented as a stacking of Gd-centred polyhedra of composition [GdSi₉]. The Re atoms form infinite chains with an Re—Re distance of 2.78163 (5) Å and isolated squares with an Re—Re distance of 2.9683 (6) Å.

Keywords: crystal structure; gadolinium; rhenium; silicon; intermetallic compound; ternary silicide.

CCDC reference: 1032373

1. Chemical context

Four structure types of composition R₂T₃Si₅ are known for the systems R–T–Si (R = rare-earth element, T = d-block element): U₂Mn₃Si₅ (Yarmolyuk et al., 1977 ) (Pearson symbol tP40, space group P4/mnc), U₂Co₃Si₅ (Akselrud et al., 1977 ) (oI40, Ibam), Nd₂Os₃Si₅ (Rizzoli et al., 2004 ) (tP48, P4/mnc) and Lu₂Co₃Si₅ (Chabot & Parthé, 1985 ) (mS40, C2/c). The structure type U₂Mn₃Si₅ has representatives in the systems R–Mn–Si (R = Y, Gd–Lu), R–Re–Si (R = Y, La–Nd, Sm, Gd–Tm), R–Fe–Si (R = Sc, Y, Sm, Gd–Lu), R–Ru–Si (R = Sm, Er, Lu), whereas the structure type U₂Co₃Si₅ has been found in the systems R–Ru–Si (R = Tb, Er), R–Co–Si (R = Sc, Y, Ce, Gd–Er), R–Rh–Si (R = Y, La, Ce, Nd, Sm, Gd–Er), R–Ir–Si (R = Y, Ce, Tb, Lu), R–Ni–Si (R = Y, Ce, Nd, Sm, Gd–Tm), R–Pt–Si (R = Ce, Sm), and R–Pd–Si (R = Ce, Sm), the structure type Nd₂Os₃Si₅ in the systems R–Os–Si (R = Nd, Eu), and the structure type Lu₂Co₃Si₅ in the systems R–Co–Si (R = Y, Tb, Dy, Lu), R–Rh–Si (R = Y, Tb, Dy) and R–Ni–Si (R = Lu) (Villars & Cenzual, 2013 ).

2. Structural commentary

The existence of the compound Gd₂Re₃Si₅ has been reported earlier (Bodak et al., 1978 ). The unit-cell parameters were determined and the structure type was assigned. A complete investigation of the crystal structure by X-ray single crystal diffraction has now been undertaken. The coordination polyhedra of the Gd atoms have 21 vertexes, whereas those of the Re atoms are cubooctahedra or 13-vertex polyhedra, and the Si atoms tricapped trigonal prisms, bicapped square antiprisms, or 11-vertex polyhedra. The U₂Mn₃Si₅-type structure is closely related to the structure type BaAl₄ and its ordered derivative CaBe₂Ge₂. In particular, the U₂Mn₃Si₅-type can be considered to be formed by one-dimensional structural fragments of the structure type CaBe₂Ge₂, running parallel to the direction [00l]. There also exists a relationship between the structure types U₂Mn₃Si₅ and W₅Si₃. Fragments which can be viewed as deformed square antiprisms are common to both structures. The crystal structure of Gd₂Re₃Si₅ can also be represented as a stacking of Gd-centred polyhedra of composition [GdSi₉], located at z = 0 and ½ (Fig. 1) (Parthé et al., 1993 ). The Re atoms form infinite chains with an Re—Re distance of 2.78163 (5) Å and isolated squares with an Re—Re distance of 2.9683 (6) Å.

Figure 1
Stacking of Gd-centred polyhedra in the structure of the compound Gd₂Re₃Si₅ with displacement ellipsoids drawn at the 99% probability level.

3. Synthesis and crystallization

An alloy of nominal atom percent composition Gd₂₀Re₃₀Si₅₀ was synthesized from the high-purity elements by arc melting on a water-cooled copper plate under a purified argon atmosphere, using titanium as a getter and a tungsten electrode. The weight loss during the sample preparation was less than 0.5% of the total mass (1 g). The alloy was placed into an Al₂O₃ crucible and inserted into a tantalum container, which was then sealed by welding, leaving the sample under an argon atmosphere. The sample, wrapped in tantalum foil, was heated to 1623 K in a muffle furnace at a rate of 200 K h⁻¹, held at this temperature for 5 h and then cooled to room temperature at a rate of 50 K h⁻¹.

4. Refinement details

A single crystal of well-defined shape was separated from the sample. The structure was solved by direct methods. The highest Fourier difference peak of 2.35 e Å⁻³ is at (0, $[1\over2]$ , $[1\over4]$ ), 0.00 Å away from atom Re2. The deepest hole (−2.44 e Å⁻³) is at (0.6045, 0.3985, 0), 1.52 Å away from the Gd atom. Details of the crystal parameters, data collection and the structure refinement details are summarized in Table 1.

Table 1
Experimental details

Crystal data
Chemical formula	Gd₂Re₃Si₅
M_r	1013.55
Crystal system, space group	Tetragonal, P4/mnc
Temperature (K)	293
a, c (Å)	10.95564 (13), 5.56326 (11)
V (Å³)	667.74 (2)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	74.55
Crystal size (mm)	0.16 × 0.10 × 0.02

Data collection
Diffractometer	Agilent Xcalibur Onyx
Absorption correction	Analytical [CrysAlis PRO (Agilent, 2012 ; analytical numeric absorption correction using a multi-faceted crystal model (Clark & Reid, 1995 )]
T_min, T_max	0.015, 0.194
No. of measured, independent and observed [I > 2σ(I)] reflections	11378, 502, 481
R_int	0.062
(sin θ/λ)_max (Å⁻¹)	0.692

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.063, 1.17
No. of reflections	502
No. of parameters	31
Δρ_max, Δρ_min (e Å⁻³)	2.35, −2.44
Computer programs: CrysAlis PRO (Agilent, 2012), SHELXS97 and SHELXL97 (Sheldrick, 2008 ), WinGX (Farrugia, 2012 ), DIAMOND (Brandenburg, 2006 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC reference: 1032373

Crystal structure: contains datablock I. DOI: 10.1107/S1600536814024234/fj2683sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814024234/fj2683Isup2.hkl

checkCIF report

Chemical context top

Four structure types of composition R₂T₃Si₅ are known for the systems R–T–Si (R = rare-earth element, T = d-element): U₂Mn₃Si₅ (Yarmolyuk et al., 1977) (Pearson symbol tP40, space group P4/mnc), U₂Co₃Si₅ (Akselrud et al., 1977) (oI40, Ibam), Nd₂Os₃Si₅ (Rizzoli et al., 2004) (tP48, P4/mnc), and Lu₂Co₃Si₅ (Chabot & Parthé, 1985) (mS40, C2/c). The structure type U₂Mn₃Si₅ has representatives in the systems R–Mn–Si (R = Y, Gd–Lu), R–Re–Si (R = Y, La–Nd, Sm, Gd–Tm), R–Fe–Si (R = Sc, Y, Sm, Gd–Lu), R–Ru–Si (R = Sm, Er, Lu), whereas the structure type U₂Co₃Si₅ has been found in the systems R–Ru–Si (R = Tb, Er), R–Co–Si (R = Sc, Y, Ce, Gd–Er), R–Rh–Si (R = Y, La, Ce, Nd, Sm, Gd–Er), R–Ir–Si (R = Y, Ce, Tb, Lu), R–Ni–Si (R = Y, Ce, Nd, Sm, Gd–Tm), R–Pt–Si (R = Ce, Sm), and R–Pd–Si (R = Ce, Sm), the structure type Nd₂Os₃Si₅ in the systems R–Os–Si (R = Nd, Eu), and the structure type Lu₂Co₃Si₅ in the systems R–Co–Si (R = Y, Tb, Dy, Lu), R–Rh–Si (R = Y, Tb, Dy), and R–Ni–Si (R = Lu) (Villars & Cenzual, 2013).

Structural commentary top

The existence of the compound Gd₂Re₃Si₅ has been reported earlier (Bodak et al., 1978). The unit-cell parameters were determined and the structure type was assigned. A complete investigation of the crystal structure by X-ray single crystal diffraction has now been undertaken. The coordination polyhedra of the Gd atoms have 21 vertexes, whereas those of the Re atoms are cubooctahedra or 13-vertex polyhedra, and the Si atoms tricapped trigonal prisms, bicapped square antiprisms, or 11-vertex polyhedra. The U₂Mn₃Si₅-type structure is closely related to the structure type BaAl₄ and its ordered derivative CaBe₂Ge₂. In particular, the U₂Mn₃Si₅-type can be considered to be formed by one-dimensional structural fragments of the structure type CaBe₂Ge₂, running parallel to the direction [00l]. There also exists a relationship between the structure types U₂Mn₃Si₅ and W₅Si₃. Fragments which can be viewed as deformed square antiprisms are common to both structures. The crystal structure of Gd₂Re₃Si₅ can also be represented as a stacking of Gd-centred polyhedra of composition [GdSi₉], located at z = 0 and ½ (Fig. 1) (Parthé et al., 1993). The Re atoms form infinite chains along [???] with an Re—Re distance of 2.78163 (5) Å and isolated squares with an Re—Re distance of 2.9683 (6) Å.

Synthesis and crystallization top

An alloy of nominal atom percent composition Gd₂₀Re₃₀Si₅₀ was synthesized from the high-purity elements by arc melting on a water-cooled copper plate under a purified argon atmosphere, using titanium as a getter and a tungsten electrode. The weight loss during the sample preparation was less than 0.5% of the total mass (1 g). The alloy was placed into an Al₂O₃ crucible and inserted into a tantalum container, which was then sealed by welding, leaving the sample under an argon atmosphere. The sample, wrapped in tantalum foil, was heated to 1623 K in a muffle furnace at a rate of 200 K h^-1, held at this temperature for 5 h and then cooled to room temperature at a rate of 50 K h^-1.

Refinement details top

A single crystal of well-defined shape was separated from the sample and investigated by X-ray crystal diffraction. The structure was solved by direct methods. A full-matrix least-squares refinement of the positional and anisotropic displacement parameters was performed on F², using the SHELXL97 program (Sheldrick, 2008). Details of the crystal parameters, data collection and the structure refinement details are summarized in Table 1.

Related literature top

For related literature, see: Akselrud et al. (1977); Bodak et al. (1978); Chabot & Parthé (1985); Clark & Reid (1995); Parthé et al. (1993); Rizzoli et al. (2004); Sheldrick (2008); Villars & Cenzual (2013); Yarmolyuk et al. (1977).

Computing details top

Data collection: CrysAlis PRO (Agilent, 2012); cell refinement: CrysAlis PRO (Agilent, 2012); data reduction: CrysAlis PRO (Agilent, 2012); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 2012); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

Stacking of Gd-centred polyhedra in the structure of the compound Gd₂Re₃Si₅ with displacement ellipsoids drawn at the 99% probability level.

Digadolinium trirhenium pentasilicide top

Crystal data top

Gd₂Re₃Si₅	D_x = 10.082 Mg m⁻³
M_r = 1013.55	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4/mnc	Cell parameters from 8564 reflections
Hall symbol: -P 4 2n	θ = 1.9–29.4°
a = 10.95564 (13) Å	µ = 74.55 mm⁻¹
c = 5.56326 (11) Å	T = 293 K
V = 667.74 (2) Å³	Irregular, grey
Z = 4	0.16 × 0.10 × 0.02 mm
F(000) = 1692

Data collection top

Agilent Xcalibur Onyx diffractometer	502 independent reflections
Radiation source: Enhance (Mo) X-ray Source	481 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.062
CCD scans	θ_max = 29.5°, θ_min = 2.6°
Absorption correction: analytical [CrysAlis PRO (Agilent, 2012; analytical numeric absorption correction using a multi-faceted crystal model (Clark & Reid, 1995)]	h = −14→14
T_min = 0.015, T_max = 0.194	k = −15→14
11378 measured reflections	l = −7→7

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.025	w = 1/[σ²(F_o²) + (0.0342P)² + 8.350P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.063	(Δ/σ)_max < 0.001
S = 1.17	Δρ_max = 2.35 e Å⁻³
502 reflections	Δρ_min = −2.44 e Å⁻³
31 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00016 (8)

Crystal data top

Gd₂Re₃Si₅	Z = 4
M_r = 1013.55	Mo Kα radiation
Tetragonal, P4/mnc	µ = 74.55 mm⁻¹
a = 10.95564 (13) Å	T = 293 K
c = 5.56326 (11) Å	0.16 × 0.10 × 0.02 mm
V = 667.74 (2) Å³

Data collection top

Agilent Xcalibur Onyx diffractometer	502 independent reflections
Absorption correction: analytical [CrysAlis PRO (Agilent, 2012; analytical numeric absorption correction using a multi-faceted crystal model (Clark & Reid, 1995)]	481 reflections with I > 2σ(I)
T_min = 0.015, T_max = 0.194	R_int = 0.062
11378 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	31 parameters
wR(F²) = 0.063	0 restraints
S = 1.17	Δρ_max = 2.35 e Å⁻³
502 reflections	Δρ_min = −2.44 e Å⁻³

Special details top

Experimental. Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by Clark & Reid (1995).

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq
Gd	0.26249 (5)	0.42271 (5)	0.0000	0.0187 (2)
Re1	0.14676 (4)	0.12315 (4)	0.0000	0.01716 (18)
Re2	0.0000	0.5000	0.2500	0.0173 (2)
Si1	0.0267 (3)	0.3149 (3)	0.0000	0.0192 (6)
Si2	0.17183 (18)	0.67183 (18)	0.2500	0.0145 (6)
Si3	0.0000	0.0000	0.2567 (9)	0.0197 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd	0.0183 (3)	0.0199 (3)	0.0179 (3)	0.0004 (2)	0.000	0.000
Re1	0.0166 (3)	0.0172 (3)	0.0177 (3)	−0.00060 (16)	0.000	0.000
Re2	0.0169 (2)	0.0169 (2)	0.0180 (3)	0.0003 (2)	0.000	0.000
Si1	0.0207 (15)	0.0184 (15)	0.0184 (14)	0.0029 (12)	0.000	0.000
Si2	0.0130 (8)	0.0130 (8)	0.0174 (13)	0.0005 (10)	−0.0025 (8)	0.0025 (8)
Si3	0.0190 (13)	0.0190 (13)	0.021 (2)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Gd—Si1	2.841 (4)	Re2—Re2^xiv	2.7816 (1)
Gd—Si1ⁱ	2.9604 (12)	Re2—Re2^viii	2.7816 (1)
Gd—Si1ⁱⁱ	2.9604 (12)	Re2—Gd^viii	3.3047 (5)
Gd—Si3ⁱⁱⁱ	3.053 (2)	Re2—Gd^xii	3.3047 (5)
Gd—Si3^iv	3.053 (2)	Re2—Gdⁱⁱ	3.3047 (5)
Gd—Re1ⁱⁱ	3.1442 (3)	Si1—Re1^xi	2.467 (4)
Gd—Re1ⁱ	3.1442 (3)	Si1—Re2^viii	2.476 (3)
Gd—Si2^v	3.163 (2)	Si1—Si2^viii	2.585 (3)
Gd—Si2^vi	3.163 (2)	Si1—Si2^xiii	2.585 (3)
Gd—Si2^vii	3.2202 (11)	Si1—Gdⁱ	2.9604 (12)
Gd—Si2	3.2202 (11)	Si1—Gdⁱⁱ	2.9604 (12)
Gd—Re2^viii	3.3047 (5)	Si2—Re1ⁱⁱⁱ	2.4837 (12)
Re1—Si1^ix	2.467 (4)	Si2—Re1^xv	2.4837 (12)
Re1—Si1	2.479 (3)	Si2—Si1^viii	2.585 (3)
Re1—Si2^vi	2.4838 (12)	Si2—Si1ⁱⁱ	2.585 (3)
Re1—Si2^v	2.4838 (12)	Si2—Si2^xvi	2.7816 (1)
Re1—Si3	2.539 (3)	Si2—Si2^vii	2.7816 (1)
Re1—Si3^x	2.539 (3)	Si2—Gdⁱⁱⁱ	3.163 (2)
Re1—Re1^xi	2.9683 (6)	Si2—Gd^xv	3.163 (2)
Re1—Re1^ix	2.9684 (6)	Si2—Gd^xii	3.2202 (11)
Re1—Gdⁱⁱ	3.1442 (3)	Si3—Re1^x	2.539 (3)
Re1—Gdⁱ	3.1442 (3)	Si3—Re1^ix	2.539 (3)
Re2—Si1ⁱⁱ	2.476 (3)	Si3—Re1^xi	2.539 (3)
Re2—Si1^xii	2.476 (3)	Si3—Si3^xvii	2.707 (9)
Re2—Si1^viii	2.476 (3)	Si3—Gdⁱⁱ	3.053 (2)
Re2—Si1	2.476 (3)	Si3—Gd^xviii	3.053 (2)
Re2—Si2^xiii	2.662 (3)	Si3—Gd^xix	3.053 (2)
Re2—Si2	2.662 (3)	Si3—Gd^xx	3.053 (2)

Si1—Gd—Si1ⁱ	79.48 (8)	Si1ⁱⁱ—Re2—Gd^xii	94.36 (7)
Si1—Gd—Si1ⁱⁱ	79.48 (8)	Si1^xii—Re2—Gd^xii	56.71 (8)
Si1ⁱ—Gd—Si1ⁱⁱ	139.97 (12)	Si1^viii—Re2—Gd^xii	59.57 (4)
Si1—Gd—Si3ⁱⁱⁱ	152.94 (8)	Si1—Re2—Gd^xii	168.30 (6)
Si1ⁱ—Gd—Si3ⁱⁱⁱ	127.50 (10)	Si2^xiii—Re2—Gd^xii	115.730 (10)
Si1ⁱⁱ—Gd—Si3ⁱⁱⁱ	77.03 (10)	Si2—Re2—Gd^xii	64.270 (10)
Si1—Gd—Si3^iv	152.94 (8)	Re2^xiv—Re2—Gd^xii	65.111 (4)
Si1ⁱ—Gd—Si3^iv	77.03 (10)	Re2^viii—Re2—Gd^xii	114.889 (4)
Si1ⁱⁱ—Gd—Si3^iv	127.50 (10)	Gd^viii—Re2—Gd^xii	74.405 (16)
Si3ⁱⁱⁱ—Gd—Si3^iv	52.64 (16)	Si1ⁱⁱ—Re2—Gdⁱⁱ	56.71 (8)
Si1—Gd—Re1ⁱⁱ	105.17 (3)	Si1^xii—Re2—Gdⁱⁱ	94.36 (7)
Si1ⁱ—Gd—Re1ⁱⁱ	172.19 (7)	Si1^viii—Re2—Gdⁱⁱ	168.29 (6)
Si1ⁱⁱ—Gd—Re1ⁱⁱ	47.80 (6)	Si1—Re2—Gdⁱⁱ	59.57 (4)
Si3ⁱⁱⁱ—Gd—Re1ⁱⁱ	48.34 (7)	Si2^xiii—Re2—Gdⁱⁱ	64.270 (10)
Si3^iv—Gd—Re1ⁱⁱ	96.88 (8)	Si2—Re2—Gdⁱⁱ	115.730 (10)
Si1—Gd—Re1ⁱ	105.17 (3)	Re2^xiv—Re2—Gdⁱⁱ	65.111 (4)
Si1ⁱ—Gd—Re1ⁱ	47.80 (6)	Re2^viii—Re2—Gdⁱⁱ	114.889 (4)
Si1ⁱⁱ—Gd—Re1ⁱ	172.19 (7)	Gd^viii—Re2—Gdⁱⁱ	128.540 (19)
Si3ⁱⁱⁱ—Gd—Re1ⁱ	96.88 (8)	Gd^xii—Re2—Gdⁱⁱ	130.223 (8)
Si3^iv—Gd—Re1ⁱ	48.34 (7)	Si1ⁱⁱ—Re2—Gd	59.57 (4)
Re1ⁱⁱ—Gd—Re1ⁱ	124.42 (2)	Si1^xii—Re2—Gd	168.30 (6)
Si1—Gd—Si2^v	81.12 (7)	Si1^viii—Re2—Gd	94.36 (7)
Si1ⁱ—Gd—Si2^v	79.33 (7)	Si1—Re2—Gd	56.71 (8)
Si1ⁱⁱ—Gd—Si2^v	129.87 (7)	Si2^xiii—Re2—Gd	115.731 (10)
Si3ⁱⁱⁱ—Gd—Si2^v	104.01 (5)	Si2—Re2—Gd	64.269 (10)
Si3^iv—Gd—Si2^v	81.50 (4)	Re2^xiv—Re2—Gd	114.888 (4)
Re1ⁱⁱ—Gd—Si2^v	95.05 (3)	Re2^viii—Re2—Gd	65.112 (4)
Re1ⁱ—Gd—Si2^v	46.377 (11)	Gd^viii—Re2—Gd	130.223 (8)
Si1—Gd—Si2^vi	81.12 (7)	Gd^xii—Re2—Gd	128.540 (19)
Si1ⁱ—Gd—Si2^vi	129.87 (7)	Gdⁱⁱ—Re2—Gd	74.406 (16)
Si1ⁱⁱ—Gd—Si2^vi	79.33 (7)	Re1^xi—Si1—Re2	122.21 (11)
Si3ⁱⁱⁱ—Gd—Si2^vi	81.50 (4)	Re1^xi—Si1—Re2^viii	122.21 (11)
Si3^iv—Gd—Si2^vi	104.01 (5)	Re2—Si1—Re2^viii	68.34 (9)
Re1ⁱⁱ—Gd—Si2^vi	46.377 (11)	Re1^xi—Si1—Re1	73.76 (10)
Re1ⁱ—Gd—Si2^vi	95.05 (3)	Re2—Si1—Re1	139.17 (9)
Si2^v—Gd—Si2^vi	52.16 (4)	Re2^viii—Si1—Re1	139.17 (9)
Si1—Gd—Si2^vii	94.12 (8)	Re1^xi—Si1—Si2^viii	58.84 (9)
Si1ⁱ—Gd—Si2^vii	49.23 (7)	Re2—Si1—Si2^viii	99.03 (11)
Si1ⁱⁱ—Gd—Si2^vii	99.13 (6)	Re2^viii—Si1—Si2^viii	63.42 (8)
Si3ⁱⁱⁱ—Gd—Si2^vii	102.67 (6)	Re1—Si1—Si2^viii	119.61 (12)
Si3^iv—Gd—Si2^vii	80.58 (5)	Re1^xi—Si1—Si2^xiii	58.84 (9)
Re1ⁱⁱ—Gd—Si2^vii	135.25 (3)	Re2—Si1—Si2^xiii	63.42 (8)
Re1ⁱ—Gd—Si2^vii	86.902 (11)	Re2^viii—Si1—Si2^xiii	99.03 (11)
Si2^v—Gd—Si2^vii	128.074 (8)	Re1—Si1—Si2^xiii	119.61 (12)
Si2^vi—Gd—Si2^vii	175.18 (3)	Si2^viii—Si1—Si2^xiii	65.09 (9)
Si1—Gd—Si2	94.12 (8)	Re1^xi—Si1—Gd	156.27 (14)
Si1ⁱ—Gd—Si2	99.13 (6)	Re2—Si1—Gd	76.51 (9)
Si1ⁱⁱ—Gd—Si2	49.23 (7)	Re2^viii—Si1—Gd	76.51 (9)
Si3ⁱⁱⁱ—Gd—Si2	80.58 (5)	Re1—Si1—Gd	82.50 (10)
Si3^iv—Gd—Si2	102.67 (6)	Si2^viii—Si1—Gd	137.86 (11)
Re1ⁱⁱ—Gd—Si2	86.902 (11)	Si2^xiii—Si1—Gd	137.86 (11)
Re1ⁱ—Gd—Si2	135.25 (3)	Re1^xi—Si1—Gdⁱ	84.88 (7)
Si2^v—Gd—Si2	175.18 (3)	Re2—Si1—Gdⁱ	141.66 (11)
Si2^vi—Gd—Si2	128.075 (8)	Re2^viii—Si1—Gdⁱ	74.27 (2)
Si2^vii—Gd—Si2	51.18 (2)	Re1—Si1—Gdⁱ	69.99 (6)
Si1—Gd—Re2^viii	46.77 (6)	Si2^viii—Si1—Gdⁱ	70.63 (3)
Si1ⁱ—Gd—Re2^viii	46.16 (6)	Si2^xiii—Si1—Gdⁱ	132.78 (12)
Si1ⁱⁱ—Gd—Re2^viii	95.63 (6)	Gd—Si1—Gdⁱ	87.06 (7)
Si3ⁱⁱⁱ—Gd—Re2^viii	149.01 (2)	Re1^xi—Si1—Gdⁱⁱ	84.88 (7)
Si3^iv—Gd—Re2^viii	118.95 (7)	Re2—Si1—Gdⁱⁱ	74.27 (2)
Re1ⁱⁱ—Gd—Re2^viii	141.358 (16)	Re2^viii—Si1—Gdⁱⁱ	141.66 (11)
Re1ⁱ—Gd—Re2^viii	92.088 (9)	Re1—Si1—Gdⁱⁱ	69.99 (6)
Si2^v—Gd—Re2^viii	103.62 (3)	Si2^viii—Si1—Gdⁱⁱ	132.78 (12)
Si2^vi—Gd—Re2^viii	127.27 (3)	Si2^xiii—Si1—Gdⁱⁱ	70.63 (3)
Si2^vii—Gd—Re2^viii	48.14 (5)	Gd—Si1—Gdⁱⁱ	87.06 (7)
Si2—Gd—Re2^viii	72.31 (3)	Gdⁱ—Si1—Gdⁱⁱ	139.97 (12)
Si1^ix—Re1—Si1	163.76 (10)	Re1ⁱⁱⁱ—Si2—Re1^xv	131.08 (12)
Si1^ix—Re1—Si2^vi	62.95 (8)	Re1ⁱⁱⁱ—Si2—Si1^viii	170.53 (14)
Si1—Re1—Si2^vi	104.06 (9)	Re1^xv—Si2—Si1^viii	58.21 (7)
Si1^ix—Re1—Si2^v	62.95 (8)	Re1ⁱⁱⁱ—Si2—Si1ⁱⁱ	58.21 (7)
Si1—Re1—Si2^v	104.06 (9)	Re1^xv—Si2—Si1ⁱⁱ	170.53 (14)
Si2^vi—Re1—Si2^v	68.11 (4)	Si1^viii—Si2—Si1ⁱⁱ	112.58 (18)
Si1^ix—Re1—Si3	96.85 (6)	Re1ⁱⁱⁱ—Si2—Re2	114.46 (6)
Si1—Re1—Si3	96.56 (7)	Re1^xv—Si2—Re2	114.46 (6)
Si2^vi—Re1—Si3	107.81 (8)	Si1^viii—Si2—Re2	56.29 (9)
Si2^v—Re1—Si3	159.37 (6)	Si1ⁱⁱ—Si2—Re2	56.29 (9)
Si1^ix—Re1—Si3^x	96.85 (6)	Re1ⁱⁱⁱ—Si2—Si2^xvi	55.947 (19)
Si1—Re1—Si3^x	96.56 (7)	Re1^xv—Si2—Si2^xvi	124.054 (19)
Si2^vi—Re1—Si3^x	159.37 (6)	Si1^viii—Si2—Si2^xvi	122.55 (5)
Si2^v—Re1—Si3^x	107.81 (8)	Si1ⁱⁱ—Si2—Si2^xvi	57.45 (5)
Si3—Re1—Si3^x	68.46 (18)	Re2—Si2—Si2^xvi	90.0
Si1^ix—Re1—Re1^xi	143.30 (8)	Re1ⁱⁱⁱ—Si2—Si2^vii	124.054 (19)
Si1—Re1—Re1^xi	52.94 (8)	Re1^xv—Si2—Si2^vii	55.947 (19)
Si2^vi—Re1—Re1^xi	141.12 (5)	Si1^viii—Si2—Si2^vii	57.45 (5)
Si2^v—Re1—Re1^xi	141.12 (5)	Si1ⁱⁱ—Si2—Si2^vii	122.55 (5)
Si3—Re1—Re1^xi	54.22 (4)	Re2—Si2—Si2^vii	90.0
Si3^x—Re1—Re1^xi	54.22 (4)	Si2^xvi—Si2—Si2^vii	180.0
Si1^ix—Re1—Re1^ix	53.30 (8)	Re1ⁱⁱⁱ—Si2—Gdⁱⁱⁱ	76.01 (6)
Si1—Re1—Re1^ix	142.94 (8)	Re1^xv—Si2—Gdⁱⁱⁱ	66.41 (5)
Si2^vi—Re1—Re1^ix	106.47 (5)	Si1^viii—Si2—Gdⁱⁱⁱ	112.27 (8)
Si2^v—Re1—Re1^ix	106.47 (5)	Si1ⁱⁱ—Si2—Gdⁱⁱⁱ	118.78 (6)
Si3—Re1—Re1^ix	54.22 (4)	Re2—Si2—Gdⁱⁱⁱ	140.83 (3)
Si3^x—Re1—Re1^ix	54.22 (4)	Si2^xvi—Si2—Gdⁱⁱⁱ	63.919 (19)
Re1^xi—Re1—Re1^ix	90.0	Si2^vii—Si2—Gdⁱⁱⁱ	116.083 (19)
Si1^ix—Re1—Gdⁱⁱ	116.473 (18)	Re1ⁱⁱⁱ—Si2—Gd^xv	66.41 (5)
Si1—Re1—Gdⁱⁱ	62.214 (12)	Re1^xv—Si2—Gd^xv	76.01 (6)
Si2^vi—Re1—Gdⁱⁱ	67.22 (4)	Si1^viii—Si2—Gd^xv	118.78 (6)
Si2^v—Re1—Gdⁱⁱ	127.12 (2)	Si1ⁱⁱ—Si2—Gd^xv	112.27 (8)
Si3—Re1—Gdⁱⁱ	63.95 (8)	Re2—Si2—Gd^xv	140.83 (3)
Si3^x—Re1—Gdⁱⁱ	123.79 (8)	Si2^xvi—Si2—Gd^xv	116.083 (19)
Re1^xi—Re1—Gdⁱⁱ	73.988 (16)	Si2^vii—Si2—Gd^xv	63.919 (19)
Re1^ix—Re1—Gdⁱⁱ	112.077 (11)	Gdⁱⁱⁱ—Si2—Gd^xv	78.35 (7)
Si1^ix—Re1—Gdⁱ	116.473 (18)	Re1ⁱⁱⁱ—Si2—Gd	79.226 (13)
Si1—Re1—Gdⁱ	62.214 (12)	Re1^xv—Si2—Gd	120.171 (7)
Si2^vi—Re1—Gdⁱ	127.12 (2)	Si1^viii—Si2—Gd	94.29 (9)
Si2^v—Re1—Gdⁱ	67.22 (4)	Si1ⁱⁱ—Si2—Gd	60.14 (5)
Si3—Re1—Gdⁱ	123.79 (8)	Re2—Si2—Gd	67.59 (5)
Si3^x—Re1—Gdⁱ	63.95 (8)	Si2^xvi—Si2—Gd	115.588 (10)
Re1^xi—Re1—Gdⁱ	73.988 (16)	Si2^vii—Si2—Gd	64.411 (10)
Re1^ix—Re1—Gdⁱ	112.077 (11)	Gdⁱⁱⁱ—Si2—Gd	148.88 (7)
Gdⁱⁱ—Re1—Gdⁱ	124.42 (2)	Gd^xv—Si2—Gd	74.63 (2)
Si1^ix—Re1—Gd	110.57 (8)	Re1ⁱⁱⁱ—Si2—Gd^xii	120.171 (7)
Si1—Re1—Gd	53.19 (8)	Re1^xv—Si2—Gd^xii	79.226 (13)
Si2^vi—Re1—Gd	60.75 (5)	Si1^viii—Si2—Gd^xii	60.14 (5)
Si2^v—Re1—Gd	60.75 (5)	Si1ⁱⁱ—Si2—Gd^xii	94.29 (9)
Si3—Re1—Gd	136.39 (6)	Re2—Si2—Gd^xii	67.59 (5)
Si3^x—Re1—Gd	136.39 (6)	Si2^xvi—Si2—Gd^xii	64.411 (10)
Re1^xi—Re1—Gd	106.13 (2)	Si2^vii—Si2—Gd^xii	115.588 (10)
Re1^ix—Re1—Gd	163.87 (2)	Gdⁱⁱⁱ—Si2—Gd^xii	74.63 (2)
Gdⁱⁱ—Re1—Gd	73.474 (15)	Gd^xv—Si2—Gd^xii	148.88 (7)
Gdⁱ—Re1—Gd	73.474 (15)	Gd—Si2—Gd^xii	135.19 (9)
Si1ⁱⁱ—Re2—Si1^xii	111.66 (9)	Re1—Si3—Re1^x	111.54 (18)
Si1ⁱⁱ—Re2—Si1^viii	120.57 (15)	Re1—Si3—Re1^ix	71.55 (9)
Si1^xii—Re2—Si1^viii	97.03 (13)	Re1^x—Si3—Re1^ix	71.55 (9)
Si1ⁱⁱ—Re2—Si1	97.03 (13)	Re1—Si3—Re1^xi	71.55 (9)
Si1^xii—Re2—Si1	120.57 (15)	Re1^x—Si3—Re1^xi	71.55 (9)
Si1^viii—Re2—Si1	111.66 (9)	Re1^ix—Si3—Re1^xi	111.54 (18)
Si1ⁱⁱ—Re2—Si2^xiii	119.72 (8)	Re1—Si3—Si3^xvii	124.23 (9)
Si1^xii—Re2—Si2^xiii	60.28 (8)	Re1^x—Si3—Si3^xvii	124.23 (9)
Si1^viii—Re2—Si2^xiii	119.72 (8)	Re1^ix—Si3—Si3^xvii	124.23 (9)
Si1—Re2—Si2^xiii	60.28 (8)	Re1^xi—Si3—Si3^xvii	124.23 (9)
Si1ⁱⁱ—Re2—Si2	60.28 (8)	Re1—Si3—Gdⁱⁱ	67.712 (11)
Si1^xii—Re2—Si2	119.72 (8)	Re1^x—Si3—Gdⁱⁱ	151.41 (5)
Si1^viii—Re2—Si2	60.28 (8)	Re1^ix—Si3—Gdⁱⁱ	129.93 (3)
Si1—Re2—Si2	119.72 (8)	Re1^xi—Si3—Gdⁱⁱ	81.779 (12)
Si2^xiii—Re2—Si2	180.0	Si3^xvii—Si3—Gdⁱⁱ	63.68 (8)
Si1ⁱⁱ—Re2—Re2^xiv	55.83 (4)	Re1—Si3—Gd^xviii	81.779 (12)
Si1^xii—Re2—Re2^xiv	55.83 (4)	Re1^x—Si3—Gd^xviii	129.93 (3)
Si1^viii—Re2—Re2^xiv	124.17 (4)	Re1^ix—Si3—Gd^xviii	67.712 (11)
Si1—Re2—Re2^xiv	124.17 (4)	Re1^xi—Si3—Gd^xviii	151.41 (5)
Si2^xiii—Re2—Re2^xiv	90.0	Si3^xvii—Si3—Gd^xviii	63.68 (8)
Si2—Re2—Re2^xiv	90.0	Gdⁱⁱ—Si3—Gd^xviii	78.66 (6)
Si1ⁱⁱ—Re2—Re2^viii	124.17 (4)	Re1—Si3—Gd^xix	151.41 (5)
Si1^xii—Re2—Re2^viii	124.17 (4)	Re1^x—Si3—Gd^xix	67.712 (11)
Si1^viii—Re2—Re2^viii	55.83 (4)	Re1^ix—Si3—Gd^xix	81.779 (12)
Si1—Re2—Re2^viii	55.83 (4)	Re1^xi—Si3—Gd^xix	129.93 (3)
Si2^xiii—Re2—Re2^viii	90.0	Si3^xvii—Si3—Gd^xix	63.68 (8)
Si2—Re2—Re2^viii	90.0	Gdⁱⁱ—Si3—Gd^xix	127.36 (16)
Re2^xiv—Re2—Re2^viii	180.0	Gd^xviii—Si3—Gd^xix	78.66 (6)
Si1ⁱⁱ—Re2—Gd^viii	168.29 (6)	Re1—Si3—Gd^xx	129.93 (3)
Si1^xii—Re2—Gd^viii	59.57 (4)	Re1^x—Si3—Gd^xx	81.779 (12)
Si1^viii—Re2—Gd^viii	56.71 (8)	Re1^ix—Si3—Gd^xx	151.41 (5)
Si1—Re2—Gd^viii	94.36 (7)	Re1^xi—Si3—Gd^xx	67.712 (11)
Si2^xiii—Re2—Gd^viii	64.270 (10)	Si3^xvii—Si3—Gd^xx	63.68 (8)
Si2—Re2—Gd^viii	115.730 (10)	Gdⁱⁱ—Si3—Gd^xx	78.66 (6)
Re2^xiv—Re2—Gd^viii	114.889 (4)	Gd^xviii—Si3—Gd^xx	127.36 (16)
Re2^viii—Re2—Gd^viii	65.111 (4)	Gd^xix—Si3—Gd^xx	78.66 (6)

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

Experimental details

Crystal data
Chemical formula	Gd₂Re₃Si₅
M_r	1013.55
Crystal system, space group	Tetragonal, P4/mnc
Temperature (K)	293
a, c (Å)	10.95564 (13), 5.56326 (11)
V (Å³)	667.74 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	74.55
Crystal size (mm)	0.16 × 0.10 × 0.02

Data collection
Diffractometer	Agilent Xcalibur Onyx diffractometer
Absorption correction	Analytical [CrysAlis PRO (Agilent, 2012; analytical numeric absorption correction using a multi-faceted crystal model (Clark & Reid, 1995)]
T_min, T_max	0.015, 0.194
No. of measured, independent and observed [I > 2σ(I)] reflections	11378, 502, 481
R_int	0.062
(sin θ/λ)_max (Å⁻¹)	0.692

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.063, 1.17
No. of reflections	502
No. of parameters	31
Δρ_max, Δρ_min (e Å⁻³)	2.35, −2.44

Computer programs: CrysAlis PRO (Agilent, 2012), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 2012), DIAMOND (Brandenburg, 2006), publCIF (Westrip, 2010).

Acknowledgements

This work was supported by the Ministry of Education and Science of Ukraine under grant No 0112U001279.

References

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