Redetermination of dysprosium trinickel from single-crystal X-ray data

Levytskyy, V.; Babizhetskyy, V.; Kotur, B.; Smetana, V.

doi:10.1107/S1600536812043747

inorganic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 68| Part 11| November 2012| Page i83

doi:10.1107/S1600536812043747

Open

access

Redetermination of dysprosium trinickel from single-crystal X-ray data

Volodymyr Levytskyy,^a ^* Volodymyr Babizhetskyy,^a Bohdan Kotur ^a and Volodymyr Smetana ^b

^aDepartment of Inorganic Chemistry, Ivan Franko National University of Lviv, Kyryla & Mefodiya street 6, 79005 Lviv, Ukraine, and ^b344 Spedding Hall, Ames Laboratory, Ames, IA 50011-3020, USA
^*Correspondence e-mail: v.levyckyy@gmail.com

(Received 28 September 2012; accepted 22 October 2012; online 27 October 2012)

The crystal structure of the title compound, DyNi₃, was redetermined from single-crystal X-ray diffraction data. In comparison with previous studies based on powder X-ray diffraction data [Lemaire & Paccard (1969 ). Bull. Soc. Fr. Minéral. Cristallogr. 92, 9–16; Tsai et al. (1974 ). J. Appl. Phys. 45, 3582–3586], the present redetermination revealed refined coordinates and anisotropic displacement parameters for all atoms. The crystal structure of DyNi₃ adopts the PuNi₃ structure type and can be derived from the CaCu₅ structure type as an intergrowth structure. The asymmetric unit contains two Dy sites (site symmetries 3m and -3) and three Ni sites (m, 3m and -3m). The two different coordination polyhedra of Dy are a Frank–Kasper polyhedron formed by four Dy and 12 Ni atoms and a pseudo-Frank–Kasper polyhedron formed by two Dy and 18 Ni atoms. The three different coordination polyhedra of Ni are Frank–Kasper icosahedra formed by five Dy and seven Ni atoms, three Dy and nine Ni atoms, and six Dy and six Ni atoms.

Related literature

For the PuNi₃ structure type, see: Cromer & Olsen (1959 ). For previous powder diffraction studies of the title compoud, see: Paccard & Pauthenet (1967 ); Lemaire & Paccard (1969); Virkar & Raman (1969 ); Buschow & van der Goot (1970 ); Yakinthos & Paccard (1972 ); Tsai et al. (1974). For related compounds, see: Virkar & Raman (1969); Buschow & van der Goot (1970); Levytskyy et al. (2012 ). For the CaCu₅ structure type, see: Haucke (1940 ); Nowotny (1942 ). For the MgCu₂ structure type, see: Friauf (1927 ); Ohba et al. (1984 ). For intergrowth structures, see: Parthé et al. (1985 ); Grin (1992 ).

Experimental

Crystal data

DyNi₃
M_r = 338.63
Trigonal, $[R \overline 3m ]$
a = 4.966 (2) Å
c = 24.37 (1) Å
V = 520.5 (4) Å³
Z = 9
Mo Kα radiation
μ = 55.52 mm⁻¹
T = 293 K
0.13 × 0.08 × 0.06 mm

Data collection

Stoe IPDS II diffractometer
Absorption correction: multi-scan (PLATON, Spek, 2009 ) T_min = 0.071, T_max = 0.182
1516 measured reflections
197 independent reflections
163 reflections with I > 2σ(I)
R_int = 0.058

Refinement

R[F² > 2σ(F²)] = 0.022
wR(F²) = 0.043
S = 1.01
197 reflections
17 parameters
Δρ_max = 2.77 e Å⁻³
Δρ_min = −1.33 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2009 ); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SIR2011 (Burla et al., 2012 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ) and WinGX (Farrugia, 1999 ); molecular graphics: DIAMOND (Brandenburg, 2006 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812043747/wm2688sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812043747/wm2688Isup2.hkl

checkCIF report

Comment top

The existence of the intermetallic phase with composition DyNi₃ has been long known before. The first structure report (Paccard & Pauthenet, 1967) of the title compound revealed isotypism with the PuNi₃ structure type (Cromer & Olsen, 1959). Lattice parameters were determined from X-ray powder diffraction data without specifying atomic coordinates (Paccard & Pauthenet, 1967; Lemaire & Paccard, 1969; Virkar & Raman, 1969; Buschow & van der Goot, 1970; Tsai et al., 1974). Yakinthos & Paccard (1972) reported crystal structure data for RNi₃ compounds (R = Pr, Nd, Tb, Dy, Tm) from powder neutron diffraction data.

The present work contains the results of the full single-crystal X-ray determination of DyNi₃, including refinement of the atomic coordinates and the temperature factors for all atoms. These results confirm the belonging to the PuNi₃ structure type in space group R3m. A view of the crystal structure of DyNi₃ is shown in Fig. 1. As has been noted previously (Yakinthos & Paccard, 1972), the crystal structure of DyNi₃ can be derived from the CaCu₅ structure type (Haucke, 1940; Nowotny, 1942). It consists of stacks of RX₅ blocks (CaCu₅-type) and R₂X₄ blocks (MgCu₂-type (Friauf, 1927; Ohba et al., 1984)). Both types have the same Kagome net of Ni atoms that allows a combination of both structural motifs along the 3-fold inversion axis. As a result, it can be considered as an intergrowth structure: R₂X₄ + RX₅ = 3RX₃ (Parthé et al., 1985; Grin, 1992).

In Fig. 2 the projection of the unit cell on the ab plane and the resulting coordination polyhedra for all atom types are shown. The coordination number for the Dy1 atom (Wyckoff site 6c, site symmetry 3m). The coordination polyhedron for this atom is a Frank-Kasper polyhedron formed by 4 Dy and 12 Ni atoms. The coordination number for the Dy2 atom (Wyckoff site 3a, site symmetry 3m) is 20. The coordination polyhedron of Dy2 is a pseudo-Frank-Kasper polyhedron formed by 2 Dy and 18 Ni atoms. Although the site symmetries for all Ni atoms are different, the coordination number for all Ni atoms is 12, with Frank-Kasper icosahedra as coordination polyhedra. The Ni1 atom (Wyckoff site 18h, site symmetry .m) is surrounded by 5 Dy atoms and 7 Ni atoms. The Ni2 atom (Wyckoff site 6c, site symmetry 3m) is surrounded by 3 Dy atoms and 9 Ni atoms. The Ni3 atom (Wyckoff site 3b, site symmetry 3m) is surrounded by 6 Dy atoms and 6 Ni atoms.

The interatomic distances in DyNi₃ are similar than those in Di₂Ni₇ (Levytskyy et al., 2012).

Related literature top

For the PuNi₃ structure type, see: Cromer & Olsen (1959). For previous powder diffraction studies of the title compoud, see: Paccard & Pauthenet (1967); Lemaire & Paccard (1969); Virkar & Raman (1969); Buschow & van der Goot (1970); Yakinthos & Paccard (1972); Tsai et al. (1974). For related compounds, see: Virkar & Raman (1969); Buschow & van der Goot (1970); Levytskyy et al. (2012). For the CaCu₅ structure type, see: Haucke (1940); Nowotny (1942). For the MgCu₂ structure type, see: Friauf (1927); Ohba et al. (1984). For intergrowth structures, see: Parthé et al. (1985); Grin (1992).

Experimental top

The sample was prepared of the powdered commercially available pure elements: sublimed bulk pieces of dysprosium metal with a claimed purity of 99.99 at.% (Alfa Aesar, Johnson Matthey) and electrolytic nickel (99.99% pure) piece (Aldrich). A mixture of the powders was compacted in stainless steel dies. The pellet was arc-melted under an argon atmosphere on a water-cooled copper hearth. The alloy button (~1 g) was turned over and remolten three times to improve homogeneity. Subsequently, the sample was annealed in an evacuated silica tube under an argon atmosphere for four weeks at 1070 K. Shiny grey irregular-shaped crystals were isolated mechanically with a help of microscope by crushing the sample.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2009); cell refinement: X-AREA (Stoe & Cie, 2009); data reduction: X-AREA (Stoe & Cie, 2009); program(s) used to solve structure: SIR2011 (Burla et al., 2012); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 1999); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. Perspective view of the crystal structure of DyNi₃. The unit cell and the blocks of RX₅ and R₂X₄ are emphasized. Atoms are represented by their anisotropic displacement ellipsoids at the 99.9% probability level
	Fig. 2. The ab projection of the unit cell and coordination polyhedra for all types of atoms in the DyNi₃ structure

Disprosium trinickel top

Crystal data top

DyNi₃	D_x = 9.723 Mg m⁻³
M_r = 338.63	Mo Kα radiation, λ = 0.71069 Å
Trigonal, R3m	Cell parameters from 1064 reflections
Hall symbol: -R 3 2"	θ = 0.8–28.4°
a = 4.966 (2) Å	µ = 55.52 mm⁻¹
c = 24.37 (1) Å	T = 293 K
V = 520.5 (4) Å³	Irregular, grey
Z = 9	0.13 × 0.08 × 0.06 mm
F(000) = 1350

Data collection top

Stoe IPDS II diffractometer	197 independent reflections
Radiation source: fine-focus sealed tube	163 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.058
ω scans	θ_max = 28.4°, θ_min = 2.5°
Absorption correction: multi-scan (PLATON, Spek, 2009)	h = −6→6
T_min = 0.071, T_max = 0.182	k = −6→6
1516 measured reflections	l = −32→30

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.022	Secondary atom site location: difference Fourier map
wR(F²) = 0.043	w = 1/[σ²(F_o²) + (0.0207P)²] where P = (F_o² + 2F_c²)/3
S = 1.01	(Δ/σ)_max < 0.001
197 reflections	Δρ_max = 2.77 e Å⁻³
17 parameters	Δρ_min = −1.33 e Å⁻³

Crystal data top

DyNi₃	Z = 9
M_r = 338.63	Mo Kα radiation
Trigonal, R3m	µ = 55.52 mm⁻¹
a = 4.966 (2) Å	T = 293 K
c = 24.37 (1) Å	0.13 × 0.08 × 0.06 mm
V = 520.5 (4) Å³

Data collection top

Stoe IPDS II diffractometer	197 independent reflections
Absorption correction: multi-scan (PLATON, Spek, 2009)	163 reflections with I > 2σ(I)
T_min = 0.071, T_max = 0.182	R_int = 0.058
1516 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.022	17 parameters
wR(F²) = 0.043	0 restraints
S = 1.01	Δρ_max = 2.77 e Å⁻³
197 reflections	Δρ_min = −1.33 e Å⁻³

Special details top

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
Ni1	0.50038 (13)	0.49962 (13)	0.08188 (5)	0.0116 (3)
Dy1	0.0000	0.0000	0.13920 (4)	0.0135 (2)
Ni2	0.0000	0.0000	0.33306 (9)	0.0143 (5)
Ni3	0.0000	0.0000	0.5000	0.0118 (7)
Dy2	0.0000	0.0000	0.0000	0.0128 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0112 (5)	0.0112 (5)	0.0141 (7)	0.0069 (6)	0.0003 (3)	−0.0003 (3)
Dy1	0.0125 (3)	0.0125 (3)	0.0157 (5)	0.00623 (15)	0.000	0.000
Ni2	0.0153 (7)	0.0153 (7)	0.0123 (12)	0.0077 (4)	0.000	0.000
Ni3	0.0115 (10)	0.0115 (10)	0.0124 (17)	0.0057 (5)	0.000	0.000
Dy2	0.0117 (4)	0.0117 (4)	0.0151 (6)	0.00584 (19)	0.000	0.000

Geometric parameters (Å, º) top

Ni1—Ni2ⁱ	2.450 (2)	Ni2—Dy2^xviii	2.8671 (12)
Ni1—Ni2ⁱⁱ	2.464 (2)	Ni2—Dy2^xv	2.8671 (12)
Ni1—Ni1ⁱⁱⁱ	2.477 (2)	Ni2—Ni2^xix	2.8671 (12)
Ni1—Ni1^iv	2.477 (2)	Ni2—Ni2^xx	2.8671 (12)
Ni1—Ni1^v	2.489 (2)	Ni2—Dy2^xxi	2.8672 (12)
Ni1—Ni1^vi	2.489 (2)	Ni2—Ni2^xxii	2.8672 (12)
Ni1—Ni3ⁱⁱ	2.5166 (14)	Ni3—Ni1^xx	2.5166 (14)
Ni1—Dy1^vii	2.8489 (11)	Ni3—Ni1^xv	2.5166 (14)
Ni1—Dy1	2.8489 (11)	Ni3—Ni1^xxiii	2.5166 (14)
Ni1—Dy1ⁱ	3.0869 (18)	Ni3—Ni1^xvii	2.5166 (14)
Ni1—Dy2	3.1855 (12)	Ni3—Ni1^xxiv	2.5166 (14)
Ni1—Dy2^vii	3.1855 (12)	Ni3—Ni1^xvi	2.5166 (14)
Dy1—Ni1^viii	2.8489 (11)	Ni3—Dy1^xx	2.9442 (11)
Dy1—Ni1^ix	2.8489 (11)	Ni3—Dy1^xv	2.9442 (11)
Dy1—Ni1^x	2.8489 (11)	Ni3—Dy1^xix	2.9442 (11)
Dy1—Ni1^vi	2.8489 (11)	Ni3—Dy1^xviii	2.9442 (11)
Dy1—Ni1^iv	2.8489 (11)	Ni3—Dy1^xxii	2.9442 (11)
Dy1—Ni3ⁱⁱ	2.9442 (11)	Ni3—Dy1^xxi	2.9442 (11)
Dy1—Ni3^xi	2.9442 (11)	Dy2—Ni2ⁱ	2.8671 (12)
Dy1—Ni3^xii	2.9442 (11)	Dy2—Ni2^xxv	2.8671 (12)
Dy1—Ni1ⁱ	3.0869 (18)	Dy2—Ni2ⁱⁱ	2.8671 (12)
Dy1—Ni1^xiii	3.0869 (18)	Dy2—Ni2^xi	2.8671 (12)
Dy1—Ni1^xiv	3.0869 (18)	Dy2—Ni2^xxvi	2.8672 (12)
Ni2—Ni1ⁱ	2.450 (2)	Dy2—Ni2^xii	2.8672 (12)
Ni2—Ni1^xiv	2.450 (2)	Dy2—Ni1^xxvii	3.1855 (12)
Ni2—Ni1^xiii	2.450 (2)	Dy2—Ni1^vi	3.1855 (12)
Ni2—Ni1^xv	2.464 (2)	Dy2—Ni1^iv	3.1855 (12)
Ni2—Ni1^xvi	2.464 (2)	Dy2—Ni1^xxviii	3.1855 (12)
Ni2—Ni1^xvii	2.464 (2)	Dy2—Ni1^viii	3.1855 (12)

Ni2ⁱ—Ni1—Ni2ⁱⁱ	71.39 (4)	Ni1^xvii—Ni2—Ni2^xix	54.07 (7)
Ni2ⁱ—Ni1—Ni1ⁱⁱⁱ	59.63 (4)	Dy2^xviii—Ni2—Ni2^xix	179.60 (14)
Ni2ⁱⁱ—Ni1—Ni1ⁱⁱⁱ	120.32 (4)	Dy2^xv—Ni2—Ni2^xix	60.0
Ni2ⁱ—Ni1—Ni1^iv	59.63 (4)	Ni1ⁱ—Ni2—Ni2^xx	107.20 (9)
Ni2ⁱⁱ—Ni1—Ni1^iv	120.32 (4)	Ni1^xiv—Ni2—Ni2^xx	107.20 (9)
Ni1ⁱⁱⁱ—Ni1—Ni1^iv	60.0	Ni1^xiii—Ni2—Ni2^xx	54.54 (7)
Ni2ⁱ—Ni1—Ni1^v	120.37 (4)	Ni1^xv—Ni2—Ni2^xx	106.72 (9)
Ni2ⁱⁱ—Ni1—Ni1^v	59.68 (4)	Ni1^xvi—Ni2—Ni2^xx	54.07 (7)
Ni1ⁱⁱⁱ—Ni1—Ni1^v	120.0	Ni1^xvii—Ni2—Ni2^xx	106.72 (9)
Ni1^iv—Ni1—Ni1^v	180.0	Dy2^xviii—Ni2—Ni2^xx	60.0
Ni2ⁱ—Ni1—Ni1^vi	120.37 (4)	Dy2^xv—Ni2—Ni2^xx	179.60 (14)
Ni2ⁱⁱ—Ni1—Ni1^vi	59.68 (4)	Ni2^xix—Ni2—Ni2^xx	119.999 (2)
Ni1ⁱⁱⁱ—Ni1—Ni1^vi	180.00 (5)	Ni1ⁱ—Ni2—Dy2^xxi	125.86 (8)
Ni1^iv—Ni1—Ni1^vi	120.0	Ni1^xiv—Ni2—Dy2^xxi	73.14 (3)
Ni1^v—Ni1—Ni1^vi	60.0	Ni1^xiii—Ni2—Dy2^xxi	73.14 (3)
Ni2ⁱ—Ni1—Ni3ⁱⁱ	179.09 (6)	Ni1^xv—Ni2—Dy2^xxi	125.53 (8)
Ni2ⁱⁱ—Ni1—Ni3ⁱⁱ	109.52 (6)	Ni1^xvi—Ni2—Dy2^xxi	72.94 (3)
Ni1ⁱⁱⁱ—Ni1—Ni3ⁱⁱ	119.63 (2)	Ni1^xvii—Ni2—Dy2^xxi	72.94 (3)
Ni1^iv—Ni1—Ni3ⁱⁱ	119.63 (2)	Dy2^xviii—Ni2—Dy2^xxi	119.999 (1)
Ni1^v—Ni1—Ni3ⁱⁱ	60.37 (2)	Dy2^xv—Ni2—Dy2^xxi	119.999 (1)
Ni1^vi—Ni1—Ni3ⁱⁱ	60.37 (2)	Ni2^xix—Ni2—Dy2^xxi	60.0
Ni2ⁱ—Ni1—Dy1^vii	113.50 (3)	Ni2^xx—Ni2—Dy2^xxi	60.0
Ni2ⁱⁱ—Ni1—Dy1^vii	113.43 (3)	Ni1ⁱ—Ni2—Ni2^xxii	54.54 (7)
Ni1ⁱⁱⁱ—Ni1—Dy1^vii	64.23 (2)	Ni1^xiv—Ni2—Ni2^xxii	107.20 (9)
Ni1^iv—Ni1—Dy1^vii	115.90 (2)	Ni1^xiii—Ni2—Ni2^xxii	107.20 (9)
Ni1^v—Ni1—Dy1^vii	64.10 (2)	Ni1^xv—Ni2—Ni2^xxii	54.07 (7)
Ni1^vi—Ni1—Dy1^vii	115.77 (2)	Ni1^xvi—Ni2—Ni2^xxii	106.72 (9)
Ni3ⁱⁱ—Ni1—Dy1^vii	66.22 (3)	Ni1^xvii—Ni2—Ni2^xxii	106.72 (9)
Ni2ⁱ—Ni1—Dy1	113.50 (3)	Dy2^xviii—Ni2—Ni2^xxii	60.0
Ni2ⁱⁱ—Ni1—Dy1	113.43 (3)	Dy2^xv—Ni2—Ni2^xxii	60.0
Ni1ⁱⁱⁱ—Ni1—Dy1	115.90 (2)	Ni2^xix—Ni2—Ni2^xxii	119.997 (2)
Ni1^iv—Ni1—Dy1	64.23 (2)	Ni2^xx—Ni2—Ni2^xxii	119.997 (2)
Ni1^v—Ni1—Dy1	115.77 (2)	Dy2^xxi—Ni2—Ni2^xxii	179.60 (14)
Ni1^vi—Ni1—Dy1	64.10 (2)	Ni1^xx—Ni3—Ni1^xv	180.00 (3)
Ni3ⁱⁱ—Ni1—Dy1	66.22 (3)	Ni1^xx—Ni3—Ni1^xxiii	59.27 (5)
Dy1^vii—Ni1—Dy1	121.28 (6)	Ni1^xv—Ni3—Ni1^xxiii	120.73 (5)
Ni2ⁱ—Ni1—Dy1ⁱ	116.67 (6)	Ni1^xx—Ni3—Ni1^xvii	120.73 (5)
Ni2ⁱⁱ—Ni1—Dy1ⁱ	171.94 (6)	Ni1^xv—Ni3—Ni1^xvii	59.27 (5)
Ni1ⁱⁱⁱ—Ni1—Dy1ⁱ	66.34 (2)	Ni1^xxiii—Ni3—Ni1^xvii	180.0
Ni1^iv—Ni1—Dy1ⁱ	66.34 (2)	Ni1^xx—Ni3—Ni1^xxiv	59.27 (5)
Ni1^v—Ni1—Dy1ⁱ	113.66 (2)	Ni1^xv—Ni3—Ni1^xxiv	120.73 (5)
Ni1^vi—Ni1—Dy1ⁱ	113.66 (2)	Ni1^xxiii—Ni3—Ni1^xxiv	59.27 (5)
Ni3ⁱⁱ—Ni1—Dy1ⁱ	62.42 (4)	Ni1^xvii—Ni3—Ni1^xxiv	120.73 (5)
Dy1^vii—Ni1—Dy1ⁱ	64.28 (3)	Ni1^xx—Ni3—Ni1^xvi	120.73 (5)
Dy1—Ni1—Dy1ⁱ	64.28 (3)	Ni1^xv—Ni3—Ni1^xvi	59.27 (5)
Ni2ⁱ—Ni1—Dy2	59.47 (3)	Ni1^xxiii—Ni3—Ni1^xvi	120.73 (5)
Ni2ⁱⁱ—Ni1—Dy2	59.37 (3)	Ni1^xvii—Ni3—Ni1^xvi	59.27 (5)
Ni1ⁱⁱⁱ—Ni1—Dy2	112.99 (2)	Ni1^xxiv—Ni3—Ni1^xvi	180.0
Ni1^iv—Ni1—Dy2	67.12 (2)	Ni1^xx—Ni3—Dy1^xx	62.314 (16)
Ni1^v—Ni1—Dy2	112.88 (2)	Ni1^xv—Ni3—Dy1^xx	117.686 (16)
Ni1^vi—Ni1—Dy2	67.01 (2)	Ni1^xxiii—Ni3—Dy1^xx	62.314 (16)
Ni3ⁱⁱ—Ni1—Dy2	120.91 (3)	Ni1^xvii—Ni3—Dy1^xx	117.686 (16)
Dy1^vii—Ni1—Dy2	170.57 (4)	Ni1^xxiv—Ni3—Dy1^xx	111.68 (4)
Dy1—Ni1—Dy2	68.15 (3)	Ni1^xvi—Ni3—Dy1^xx	68.32 (4)
Dy1ⁱ—Ni1—Dy2	123.75 (3)	Ni1^xx—Ni3—Dy1^xv	117.686 (16)
Ni2ⁱ—Ni1—Dy2^vii	59.47 (3)	Ni1^xv—Ni3—Dy1^xv	62.314 (16)
Ni2ⁱⁱ—Ni1—Dy2^vii	59.37 (3)	Ni1^xxiii—Ni3—Dy1^xv	117.686 (16)
Ni1ⁱⁱⁱ—Ni1—Dy2^vii	67.12 (2)	Ni1^xvii—Ni3—Dy1^xv	62.314 (16)
Ni1^iv—Ni1—Dy2^vii	112.99 (2)	Ni1^xxiv—Ni3—Dy1^xv	68.32 (4)
Ni1^v—Ni1—Dy2^vii	67.01 (2)	Ni1^xvi—Ni3—Dy1^xv	111.68 (4)
Ni1^vi—Ni1—Dy2^vii	112.88 (2)	Dy1^xx—Ni3—Dy1^xv	180.0
Ni3ⁱⁱ—Ni1—Dy2^vii	120.91 (3)	Ni1^xx—Ni3—Dy1^xix	62.314 (16)
Dy1^vii—Ni1—Dy2^vii	68.15 (3)	Ni1^xv—Ni3—Dy1^xix	117.686 (16)
Dy1—Ni1—Dy2^vii	170.57 (4)	Ni1^xxiii—Ni3—Dy1^xix	111.68 (4)
Dy1ⁱ—Ni1—Dy2^vii	123.75 (3)	Ni1^xvii—Ni3—Dy1^xix	68.32 (4)
Dy2—Ni1—Dy2^vii	102.42 (5)	Ni1^xxiv—Ni3—Dy1^xix	62.314 (16)
Ni1^viii—Dy1—Ni1^ix	51.80 (5)	Ni1^xvi—Ni3—Dy1^xix	117.686 (16)
Ni1^viii—Dy1—Ni1^x	51.54 (5)	Dy1^xx—Ni3—Dy1^xix	114.993 (13)
Ni1^ix—Dy1—Ni1^x	98.01 (4)	Dy1^xv—Ni3—Dy1^xix	65.007 (13)
Ni1^viii—Dy1—Ni1	121.28 (6)	Ni1^xx—Ni3—Dy1^xviii	117.686 (16)
Ni1^ix—Dy1—Ni1	98.01 (4)	Ni1^xv—Ni3—Dy1^xviii	62.314 (16)
Ni1^x—Dy1—Ni1	98.01 (4)	Ni1^xxiii—Ni3—Dy1^xviii	68.32 (4)
Ni1^viii—Dy1—Ni1^vi	98.01 (4)	Ni1^xvii—Ni3—Dy1^xviii	111.68 (4)
Ni1^ix—Dy1—Ni1^vi	51.54 (5)	Ni1^xxiv—Ni3—Dy1^xviii	117.686 (16)
Ni1^x—Dy1—Ni1^vi	121.28 (6)	Ni1^xvi—Ni3—Dy1^xviii	62.314 (16)
Ni1—Dy1—Ni1^vi	51.80 (5)	Dy1^xx—Ni3—Dy1^xviii	65.007 (13)
Ni1^viii—Dy1—Ni1^iv	98.01 (4)	Dy1^xv—Ni3—Dy1^xviii	114.993 (13)
Ni1^ix—Dy1—Ni1^iv	121.28 (6)	Dy1^xix—Ni3—Dy1^xviii	180.00 (3)
Ni1^x—Dy1—Ni1^iv	51.80 (5)	Ni1^xx—Ni3—Dy1^xxii	111.68 (4)
Ni1—Dy1—Ni1^iv	51.54 (5)	Ni1^xv—Ni3—Dy1^xxii	68.32 (4)
Ni1^vi—Dy1—Ni1^iv	98.01 (4)	Ni1^xxiii—Ni3—Dy1^xxii	62.314 (16)
Ni1^viii—Dy1—Ni3ⁱⁱ	147.89 (3)	Ni1^xvii—Ni3—Dy1^xxii	117.686 (16)
Ni1^ix—Dy1—Ni3ⁱⁱ	96.33 (2)	Ni1^xxiv—Ni3—Dy1^xxii	62.314 (16)
Ni1^x—Dy1—Ni3ⁱⁱ	147.89 (3)	Ni1^xvi—Ni3—Dy1^xxii	117.686 (16)
Ni1—Dy1—Ni3ⁱⁱ	51.46 (3)	Dy1^xx—Ni3—Dy1^xxii	114.992 (13)
Ni1^vi—Dy1—Ni3ⁱⁱ	51.46 (3)	Dy1^xv—Ni3—Dy1^xxii	65.008 (13)
Ni1^iv—Dy1—Ni3ⁱⁱ	96.33 (2)	Dy1^xix—Ni3—Dy1^xxii	114.992 (13)
Ni1^viii—Dy1—Ni3^xi	51.46 (3)	Dy1^xviii—Ni3—Dy1^xxii	65.008 (13)
Ni1^ix—Dy1—Ni3^xi	51.46 (3)	Ni1^xx—Ni3—Dy1^xxi	68.32 (4)
Ni1^x—Dy1—Ni3^xi	96.33 (2)	Ni1^xv—Ni3—Dy1^xxi	111.68 (4)
Ni1—Dy1—Ni3^xi	147.89 (3)	Ni1^xxiii—Ni3—Dy1^xxi	117.686 (16)
Ni1^vi—Dy1—Ni3^xi	96.33 (2)	Ni1^xvii—Ni3—Dy1^xxi	62.314 (16)
Ni1^iv—Dy1—Ni3^xi	147.89 (3)	Ni1^xxiv—Ni3—Dy1^xxi	117.686 (16)
Ni3ⁱⁱ—Dy1—Ni3^xi	114.993 (13)	Ni1^xvi—Ni3—Dy1^xxi	62.314 (16)
Ni1^viii—Dy1—Ni3^xii	96.33 (2)	Dy1^xx—Ni3—Dy1^xxi	65.008 (13)
Ni1^ix—Dy1—Ni3^xii	147.89 (3)	Dy1^xv—Ni3—Dy1^xxi	114.992 (13)
Ni1^x—Dy1—Ni3^xii	51.46 (3)	Dy1^xix—Ni3—Dy1^xxi	65.008 (13)
Ni1—Dy1—Ni3^xii	96.33 (2)	Dy1^xviii—Ni3—Dy1^xxi	114.992 (13)
Ni1^vi—Dy1—Ni3^xii	147.89 (3)	Dy1^xxii—Ni3—Dy1^xxi	180.00 (3)
Ni1^iv—Dy1—Ni3^xii	51.46 (3)	Ni2ⁱ—Dy2—Ni2^xxv	120.0
Ni3ⁱⁱ—Dy1—Ni3^xii	114.992 (13)	Ni2ⁱ—Dy2—Ni2ⁱⁱ	60.0
Ni3^xi—Dy1—Ni3^xii	114.992 (13)	Ni2^xxv—Dy2—Ni2ⁱⁱ	180.0
Ni1^viii—Dy1—Ni1ⁱ	115.72 (3)	Ni2ⁱ—Dy2—Ni2^xi	180.0
Ni1^ix—Dy1—Ni1ⁱ	141.67 (2)	Ni2^xxv—Dy2—Ni2^xi	60.0
Ni1^x—Dy1—Ni1ⁱ	94.88 (4)	Ni2ⁱⁱ—Dy2—Ni2^xi	120.0
Ni1—Dy1—Ni1ⁱ	115.72 (3)	Ni2ⁱ—Dy2—Ni2^xxvi	120.0
Ni1^vi—Dy1—Ni1ⁱ	141.67 (2)	Ni2^xxv—Dy2—Ni2^xxvi	120.0
Ni1^iv—Dy1—Ni1ⁱ	94.88 (4)	Ni2ⁱⁱ—Dy2—Ni2^xxvi	60.0
Ni3ⁱⁱ—Dy1—Ni1ⁱ	91.38 (3)	Ni2^xi—Dy2—Ni2^xxvi	60.0
Ni3^xi—Dy1—Ni1ⁱ	91.38 (3)	Ni2ⁱ—Dy2—Ni2^xii	60.0
Ni3^xii—Dy1—Ni1ⁱ	49.26 (2)	Ni2^xxv—Dy2—Ni2^xii	60.0
Ni1^viii—Dy1—Ni1^xiii	141.67 (2)	Ni2ⁱⁱ—Dy2—Ni2^xii	120.0
Ni1^ix—Dy1—Ni1^xiii	115.72 (3)	Ni2^xi—Dy2—Ni2^xii	120.0
Ni1^x—Dy1—Ni1^xiii	141.67 (2)	Ni2^xxvi—Dy2—Ni2^xii	180.0
Ni1—Dy1—Ni1^xiii	94.88 (4)	Ni2ⁱ—Dy2—Ni1	47.39 (4)
Ni1^vi—Dy1—Ni1^xiii	94.88 (4)	Ni2^xxv—Dy2—Ni1	132.30 (4)
Ni1^iv—Dy1—Ni1^xiii	115.72 (3)	Ni2ⁱⁱ—Dy2—Ni1	47.70 (4)
Ni3ⁱⁱ—Dy1—Ni1^xiii	49.26 (2)	Ni2^xi—Dy2—Ni1	132.61 (4)
Ni3^xi—Dy1—Ni1^xiii	91.38 (3)	Ni2^xxvi—Dy2—Ni1	89.97 (4)
Ni3^xii—Dy1—Ni1^xiii	91.39 (3)	Ni2^xii—Dy2—Ni1	90.03 (4)
Ni1ⁱ—Dy1—Ni1^xiii	47.32 (4)	Ni2ⁱ—Dy2—Ni1^xxvii	132.61 (4)
Ni1^viii—Dy1—Ni1^xiv	94.88 (4)	Ni2^xxv—Dy2—Ni1^xxvii	47.70 (4)
Ni1^ix—Dy1—Ni1^xiv	94.88 (4)	Ni2ⁱⁱ—Dy2—Ni1^xxvii	132.30 (4)
Ni1^x—Dy1—Ni1^xiv	115.72 (3)	Ni2^xi—Dy2—Ni1^xxvii	47.39 (4)
Ni1—Dy1—Ni1^xiv	141.67 (2)	Ni2^xxvi—Dy2—Ni1^xxvii	90.03 (4)
Ni1^vi—Dy1—Ni1^xiv	115.72 (3)	Ni2^xii—Dy2—Ni1^xxvii	89.97 (4)
Ni1^iv—Dy1—Ni1^xiv	141.67 (2)	Ni1—Dy2—Ni1^xxvii	180.00 (3)
Ni3ⁱⁱ—Dy1—Ni1^xiv	91.38 (3)	Ni2ⁱ—Dy2—Ni1^vi	89.97 (4)
Ni3^xi—Dy1—Ni1^xiv	49.26 (2)	Ni2^xxv—Dy2—Ni1^vi	132.30 (4)
Ni3^xii—Dy1—Ni1^xiv	91.39 (3)	Ni2ⁱⁱ—Dy2—Ni1^vi	47.70 (4)
Ni1ⁱ—Dy1—Ni1^xiv	47.32 (4)	Ni2^xi—Dy2—Ni1^vi	90.03 (4)
Ni1^xiii—Dy1—Ni1^xiv	47.32 (4)	Ni2^xxvi—Dy2—Ni1^vi	47.39 (4)
Ni1ⁱ—Ni2—Ni1^xiv	60.75 (7)	Ni2^xii—Dy2—Ni1^vi	132.61 (4)
Ni1ⁱ—Ni2—Ni1^xiii	60.75 (7)	Ni1—Dy2—Ni1^vi	45.99 (4)
Ni1^xiv—Ni2—Ni1^xiii	60.75 (7)	Ni1^xxvii—Dy2—Ni1^vi	134.01 (4)
Ni1ⁱ—Ni2—Ni1^xv	108.61 (4)	Ni2ⁱ—Dy2—Ni1^iv	47.39 (4)
Ni1^xiv—Ni2—Ni1^xv	146.078 (19)	Ni2^xxv—Dy2—Ni1^iv	89.97 (4)
Ni1^xiii—Ni2—Ni1^xv	146.078 (19)	Ni2ⁱⁱ—Dy2—Ni1^iv	90.03 (4)
Ni1ⁱ—Ni2—Ni1^xvi	146.078 (19)	Ni2^xi—Dy2—Ni1^iv	132.61 (4)
Ni1^xiv—Ni2—Ni1^xvi	146.077 (19)	Ni2^xxvi—Dy2—Ni1^iv	132.30 (4)
Ni1^xiii—Ni2—Ni1^xvi	108.61 (4)	Ni2^xii—Dy2—Ni1^iv	47.70 (4)
Ni1^xv—Ni2—Ni1^xvi	60.65 (7)	Ni1—Dy2—Ni1^iv	45.77 (4)
Ni1ⁱ—Ni2—Ni1^xvii	146.078 (19)	Ni1^xxvii—Dy2—Ni1^iv	134.23 (4)
Ni1^xiv—Ni2—Ni1^xvii	108.61 (4)	Ni1^vi—Dy2—Ni1^iv	84.91 (3)
Ni1^xiii—Ni2—Ni1^xvii	146.077 (19)	Ni2ⁱ—Dy2—Ni1^xxviii	90.03 (4)
Ni1^xv—Ni2—Ni1^xvii	60.65 (7)	Ni2^xxv—Dy2—Ni1^xxviii	47.70 (4)
Ni1^xvi—Ni2—Ni1^xvii	60.65 (7)	Ni2ⁱⁱ—Dy2—Ni1^xxviii	132.30 (4)
Ni1ⁱ—Ni2—Dy2^xviii	73.14 (3)	Ni2^xi—Dy2—Ni1^xxviii	89.97 (4)
Ni1^xiv—Ni2—Dy2^xviii	125.86 (8)	Ni2^xxvi—Dy2—Ni1^xxviii	132.61 (4)
Ni1^xiii—Ni2—Dy2^xviii	73.14 (3)	Ni2^xii—Dy2—Ni1^xxviii	47.39 (4)
Ni1^xv—Ni2—Dy2^xviii	72.94 (3)	Ni1—Dy2—Ni1^xxviii	134.01 (4)
Ni1^xvi—Ni2—Dy2^xviii	72.94 (3)	Ni1^xxvii—Dy2—Ni1^xxviii	45.99 (4)
Ni1^xvii—Ni2—Dy2^xviii	125.53 (8)	Ni1^vi—Dy2—Ni1^xxviii	180.00 (5)
Ni1ⁱ—Ni2—Dy2^xv	73.14 (3)	Ni1^iv—Dy2—Ni1^xxviii	95.09 (3)
Ni1^xiv—Ni2—Dy2^xv	73.14 (3)	Ni2ⁱ—Dy2—Ni1^viii	132.30 (4)
Ni1^xiii—Ni2—Dy2^xv	125.86 (8)	Ni2^xxv—Dy2—Ni1^viii	47.39 (4)
Ni1^xv—Ni2—Dy2^xv	72.94 (3)	Ni2ⁱⁱ—Dy2—Ni1^viii	132.61 (4)
Ni1^xvi—Ni2—Dy2^xv	125.53 (8)	Ni2^xi—Dy2—Ni1^viii	47.70 (4)
Ni1^xvii—Ni2—Dy2^xv	72.94 (3)	Ni2^xxvi—Dy2—Ni1^viii	89.97 (4)
Dy2^xviii—Ni2—Dy2^xv	120.000 (1)	Ni2^xii—Dy2—Ni1^viii	90.03 (4)
Ni1ⁱ—Ni2—Ni2^xix	107.20 (9)	Ni1—Dy2—Ni1^viii	102.42 (5)
Ni1^xiv—Ni2—Ni2^xix	54.54 (7)	Ni1^xxvii—Dy2—Ni1^viii	77.58 (5)
Ni1^xiii—Ni2—Ni2^xix	107.20 (9)	Ni1^vi—Dy2—Ni1^viii	84.91 (3)
Ni1^xv—Ni2—Ni2^xix	106.72 (9)	Ni1^iv—Dy2—Ni1^viii	84.91 (3)
Ni1^xvi—Ni2—Ni2^xix	106.72 (9)	Ni1^xxviii—Dy2—Ni1^viii	95.09 (3)

Symmetry codes: (i) −x+2/3, −y+1/3, −z+1/3; (ii) x+1/3, y+2/3, z−1/3; (iii) −x+y+1, −x+1, z; (iv) −y+1, x−y, z; (v) −y+1, x−y+1, z; (vi) −x+y, −x+1, z; (vii) x+1, y+1, z; (viii) x−1, y−1, z; (ix) −y, x−y, z; (x) −x+y, −x, z; (xi) x−2/3, y−1/3, z−1/3; (xii) x+1/3, y−1/3, z−1/3; (xiii) y−1/3, −x+y+1/3, −z+1/3; (xiv) x−y−1/3, x−2/3, −z+1/3; (xv) x−1/3, y−2/3, z+1/3; (xvi) −y+2/3, x−y+1/3, z+1/3; (xvii) −x+y−1/3, −x+1/3, z+1/3; (xviii) x+2/3, y+1/3, z+1/3; (xix) −x−2/3, −y−1/3, −z+2/3; (xx) −x+1/3, −y+2/3, −z+2/3; (xxi) x−1/3, y+1/3, z+1/3; (xxii) −x+1/3, −y−1/3, −z+2/3; (xxiii) x−y+1/3, x−1/3, −z+2/3; (xxiv) y−2/3, −x+y−1/3, −z+2/3; (xxv) −x−1/3, −y−2/3, −z+1/3; (xxvi) −x−1/3, −y+1/3, −z+1/3; (xxvii) −x, −y, −z; (xxviii) x−y, x−1, −z.

Experimental details

Crystal data
Chemical formula	DyNi₃
M_r	338.63
Crystal system, space group	Trigonal, R3m
Temperature (K)	293
a, c (Å)	4.966 (2), 24.37 (1)
V (Å³)	520.5 (4)
Z	9
Radiation type	Mo Kα
µ (mm⁻¹)	55.52
Crystal size (mm)	0.13 × 0.08 × 0.06

Data collection
Diffractometer	Stoe IPDS II diffractometer
Absorption correction	Multi-scan (PLATON, Spek, 2009)
T_min, T_max	0.071, 0.182
No. of measured, independent and observed [I > 2σ(I)] reflections	1516, 197, 163
R_int	0.058
(sin θ/λ)_max (Å⁻¹)	0.670

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.022, 0.043, 1.01
No. of reflections	197
No. of parameters	17
Δρ_max, Δρ_min (e Å⁻³)	2.77, −1.33

Computer programs: X-AREA (Stoe & Cie, 2009), SIR2011 (Burla et al., 2012), SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 1999), DIAMOND (Brandenburg, 2006), publCIF (Westrip, 2010).

References

Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Mallamo, M., Mazzone, A., Polidori, G. & Spagna, R. (2012). J. Appl. Cryst. 45, 357–361. Web of Science CrossRef CAS IUCr Journals Google Scholar
Buschow, K. H. J. & van der Goot, A. S. (1970). J. Less Common Met. 22, 419–428. CrossRef CAS Google Scholar
Cromer, D. T. & Olsen, C. E. (1959). Acta Cryst. 12, 689–694. CrossRef CAS IUCr Journals Web of Science Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Friauf, J. B. (1927). J. Am. Chem. Soc. 49, 3107–3114. CrossRef CAS Google Scholar
Grin, Yu. (1992). Modern Perspectives in Inorganic Crystal Chemistry, edited by E. Parthé, pp. 77–95. Dordrecht: Kluwer Academic Publishers. Google Scholar
Haucke, W. (1940). Z. Anorg. Allg. Chem. 244, 17–22. CrossRef CAS Google Scholar
Lemaire, R. & Paccard, D. (1969). Bull. Soc. Fr. Minéral. Cristallogr. 92, 9–16. CAS Google Scholar
Levytskyy, V., Babizhetskyy, V., Kotur, B. & Smetana, V. (2012). Acta Cryst. E68, i20. CrossRef IUCr Journals Google Scholar
Nowotny, H. (1942). Z. Metallkd. 34, 247–253. CAS Google Scholar
Ohba, T., Kitano, Y. & Komura, Y. (1984). Acta Cryst. C40, 1–5. CrossRef CAS Web of Science IUCr Journals Google Scholar
Paccard, D. & Pauthenet, R. (1967). Compt. Rend. Sci. Ser. B. 264, 1056–1059. Google Scholar
Parthé, E., Chabot, B. A. & Censual, K. (1985). Chimia, 39, 164–174. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie. (2009). X-AREA. Stoe & Cie, Darmstadt, Germany. Google Scholar
Tsai, S. C., Narasimhan, K. S. V. L., Kemesh, C. J. & Butera, R. A. (1974). J. Appl. Phys. 45, 3582–3586. CrossRef CAS Web of Science Google Scholar
Virkar, A. V. & Raman, A. (1969). J. Less Common Met. 18, 59–66. CrossRef CAS Web of Science Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yakinthos, J. & Paccard, D. (1972). Solid State Commun. 10, 989–993. CrossRef CAS Web of Science Google Scholar