Zr3NiSb7: a new anti­mony-enriched ZrSb2 derivative

Romaka, V.; Tkachuk, A.; Romaka, L.

doi:10.1107/S1600536808020278

inorganic compounds

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Volume 64| Part 8| August 2008| Page i47

doi:10.1107/S1600536808020278

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Zr₃NiSb₇: a new antimony-enriched ZrSb₂ derivative

V. Romaka,^a ^* A. Tkachuk ^b and L. Romaka ^a

^aDepartment of Inorganic Chemistry, Ivan Franko National University of Lviv, Kyryla i Mefodiya Street 6, 79005 Lviv, Ukraine, and ^bDepartment of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G 2G2
^*Correspondence e-mail: romakav@yahoo.com

(Received 27 June 2008; accepted 2 July 2008; online 5 July 2008)

Single crystals of trizirconium nickel heptaantimonide were synthesized from the constituent elements by arc-melting. The compound crystallizes in a unique structure type and belongs to the family of two-layer structures. All crystallographically unique atoms (3 × Zr, 1 × Ni and 7 × Sb) are located at sites with m symmetry. The structure contains `Zr₂Ni₂Sb₅' and `Zr₄Sb₉' fragments and might be described as a new ZrSb₂ derivative with a high Sb content.

Related literature

The structure of ZrSb₂ was described by Garcia & Corbett (1988 ). For related antimonides, see: Romaka et al. (2007 ); Tkachuk et al. (2007 ). For related literature, see: Emsley (1991 ).

Experimental

Crystal data

Zr₃NiSb₇
M_r = 1184.62
Orthorhombic, P n m a
a = 17.5165 (19) Å
b = 3.9266 (4) Å
c = 14.3968 (15) Å
V = 990.22 (18) Å³
Z = 4
Mo Kα radiation
μ = 23.56 mm⁻¹
T = 295 (2) K
0.37 × 0.06 × 0.04 mm

Data collection

Bruker SMART 1000 diffractometer
Absorption correction: numerical (SHELXTL; Sheldrick, 2008 ) T_min = 0.057, T_max = 0.426
11118 measured reflections
1722 independent reflections
1500 reflections with I > 2σ(I)
R_int = 0.043

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.053
S = 1.18
1722 reflections
68 parameters
Δρ_max = 2.12 e Å⁻³
Δρ_min = −2.89 e Å⁻³

Table 1
Selected bond lengths (Å)

Zr1—Sb4ⁱ	2.9620 (6)
Zr1—Sb6	2.9876 (8)
Zr1—Sb1ⁱⁱ	3.0669 (8)
Zr1—Sb3ⁱⁱⁱ	3.0720 (7)
Zr1—Sb7ⁱⁱⁱ	3.0960 (6)
Zr1—Sb5	3.1324 (8)
Zr2—Sb6^iv	2.9478 (6)
Zr2—Sb4ⁱⁱⁱ	2.9499 (6)
Zr2—Sb2^iv	2.9604 (6)
Zr2—Sb2ⁱⁱ	3.0029 (8)
Zr2—Sb5	3.0044 (8)
Zr3—Sb1^iv	2.9569 (6)
Zr3—Sb3^iv	2.9944 (7)
Zr3—Sb5^iv	2.9958 (6)
Zr3—Sb6^v	2.9975 (8)
Zr3—Sb3^vi	3.1616 (9)
Ni1—Sb7	2.5728 (10)
Ni1—Sb2^iv	2.5875 (7)
Ni1—Sb1^iv	2.6140 (7)
Ni1—Sb4^vi	2.7141 (10)
Sb1—Sb2	3.1998 (8)
Sb1—Sb3^vii	3.2645 (6)
Sb1—Sb4^viii	3.2981 (6)
Sb2—Sb2^ix	3.2250 (7)
Sb2—Sb4^viii	3.3111 (6)
Sb5—Sb7ⁱⁱⁱ	3.1380 (6)
Sb5—Sb6^iv	3.1387 (6)
Sb6—Sb7ⁱ	3.1393 (6)
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y+1, z-{\script{1\over 2}}]$ ; (ii) $[x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]$ ; (iii) $[-x+{\script{1\over 2}}, -y, z-{\script{1\over 2}}]$ ; (iv) $[-x+{\script{1\over 2}}, -y, z+{\script{1\over 2}}]$ ; (v) x, y, z+1; (vi) $[x+{\script{1\over 2}}, y, -z+{\script{3\over 2}}]$ ; (vii) -x, -y+1, -z+1; (viii) -x, -y, -z+1; (ix) -x, -y, -z.

Data collection: SMART (Bruker, 2000 ); cell refinement: SAINT-Plus (Bruker, 2000); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808020278/wm2182sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808020278/wm2182Isup2.hkl

checkCIF report

Comment top

Antimony based intermetallics attract interest due to interesting thermoelectric properties of some phases, e.g. antimonides with MgAgAs and Y₃Au₃Sb₄ type structures. The investigation of new intermetallic phases is useful for the development of new materials, and the accurate determination of their crystal structures is a basic requirement for a better understanding of the corresponding physical properties.

Investigation of the Zr–Ni–Sb ternary system revealed the presence of several compounds in the Sb-enriched area (Romaka et al., 2007), including the new title antimonide with composition Zr₂₇Ni₉Sb₆₄ (in %_at). Interatomic distances (Table 1) between Sb atoms are in good agreement with the sum of the atomic radius (Emsley, 1991), whereas the majority of Zr—Sb and all Ni—Sb distances are somewhat shortened. Such shortening may be explained by partial covalent bonding which appears to be significant between Ni—Sb atoms because their contact distances are rather close to the sum of their covalent radii (2.56 Å). As the majority of ternary intermetallics are constructed from the fragments of their most stable binary compounds, the structure analysis of the antimonides Zr₃NiSb₇ and the already known Zr₂NiSb₃ (Tkachuk et al., 2007) in the Sb-enriched area shows that both can be derived from the binary compound ZrSb₂ (Garcia & Corbett, 1988), which crystallizes in the PbCl₂ structure type.

Zr₃NiSb₇ belongs to the family of two-layer structures. It may be represented as a net of trigonal prisms formed by Sb atoms that are bridged by nickel atoms (Fig. 1a). Such an arrangement is very similar to that in the binary ZrSb₂ structure (Fig. 1b). The coordination polyhedra are distorted tri-capped trigonal prisms for the Zr atoms, and distorted octahedra for Ni atoms. In an alternative description, the Zr₃NiSb₇ structure contains fragments of the hypothetical "Zr₂Ni₂Sb₅" and "Zr₄Sb₉" structures (Fig. 2) which are so far unknown for the ternary Zr–Ni–Sb or binary Zr–Sb systems. The main feature of the Zr₃NiSb₇ structure is the absence of covalent bonding between antimony atoms in contrast to the ZrSb₂ structure. The general conclusion is that the presence of Ni atoms intensifies the interaction between Zr/Ni and Sb and, at the same time, reduces the bonding between Sb atoms. One may speculate that the composition of the Zr₃NiSb₇ compound may be the boundary limit of some solid solutions based on ZrSb₂. However, the detailed study of the phase equilibria in the Zr–Ni–Sb system did not show a formation of any substitutional or interstitial solid solution. Moreover, the diffraction patterns of Zr₃NiSb₇ and ZrSb₂ are rather different.

Related literature top

The structure of ZrSb₂ was described by Garcia & Corbett (1988). For related antimonides, see: Romaka et al. (2007); Tkachuk et al. (2007). For related literature, see: Emsley (1991).

Experimental top

A sample with nominal composition Zr₃₀Ni₁₀Sb₆₀ was prepared by arc-melting the constituent elements Zr (99.99 wt.%), Ni (99.99 wt.%), and Sb (99.99 wt.%) on a water-cooled copper hearth under a protective Ti-gettered argon atmosphere. 5 wt.% excess of Sb was required to compensate the evaporative loss during arc-melting. The ingot was annealed at 870 K for 720 h in an evacuated silica ampoule, and finally quenched in cold water. A crystal of the title compound suitable for single-crystal X-ray diffraction was extracted directly from the annealed sample. The chemical composition of the crystal was determined on the basis of an energy dispersive X-ray spectroscopical analysis using a Hitachi S-2700 scanning electron microscope. The result of the analysis is in good aggreement with the composition calculated from the structural refinement: Measured: 24.5 (8) %_at Zr, 11.3 (6) %_at Ni, 64.2 (16) %_at Sb; calculated Zr 27 %_at, Ni 9%_at, Sb 64 %_at.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT-Plus (Bruker, 2000); data reduction: SAINT-Plus (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. (a). Projection of the Zr₃NiSb₇ structure onto the (010) plane with displacement ellipsoids drawn at the 95% probability level. [Symmetry codes: (i) 0.5 - x, 1 - y, -1/2 + z; (iv) 0.5 - x, -y, 0.5 - z; (vi) 1/2 + x, y, 1.5 - z]; (b) Projection of the ZrSb₂ structure onto the (010) plane.
	Fig. 2. The stacked "Zr₂Ni₂Sb₅" and "Zr₄Sb₉" fragments in the Zr₃NiSb₇ structure.

trizirconium nickel heptaantimonide top

Crystal data top

Zr₃NiSb₇	F(000) = 2020
M_r = 1184.62	D_x = 7.946 Mg m⁻³
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 4956 reflections
a = 17.5165 (19) Å	θ = 2.3–33.1°
b = 3.9266 (4) Å	µ = 23.56 mm⁻¹
c = 14.3968 (15) Å	T = 295 K
V = 990.22 (18) Å³	Needle, silver
Z = 4	0.37 × 0.06 × 0.04 mm

Data collection top

Bruker SMART 1000 diffractometer	1722 independent reflections
Radiation source: fine-focus sealed tube	1500 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.044
ϕ and ω scans	θ_max = 30.5°, θ_min = 2.3°
Absorption correction: numerical (SHELXTL; Sheldrick, 2008)	h = −25→25
T_min = 0.057, T_max = 0.426	k = −5→5
11118 measured reflections	l = −20→20

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)] = 0.024	w = 1/[σ²(F_o²) + (0.0223P)² + 1.1518P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.054	(Δ/σ)_max = 0.001
S = 1.18	Δρ_max = 2.12 e Å⁻³
1722 reflections	Δρ_min = −2.89 e Å⁻³
68 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00069 (5)

Crystal data top

Zr₃NiSb₇	V = 990.22 (18) Å³
M_r = 1184.62	Z = 4
Orthorhombic, Pnma	Mo Kα radiation
a = 17.5165 (19) Å	µ = 23.56 mm⁻¹
b = 3.9266 (4) Å	T = 295 K
c = 14.3968 (15) Å	0.37 × 0.06 × 0.04 mm

Data collection top

Bruker SMART 1000 diffractometer	1722 independent reflections
Absorption correction: numerical (SHELXTL; Sheldrick, 2008)	1500 reflections with I > 2σ(I)
T_min = 0.057, T_max = 0.426	R_int = 0.044
11118 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	68 parameters
wR(F²) = 0.054	0 restraints
S = 1.18	Δρ_max = 2.12 e Å⁻³
1722 reflections	Δρ_min = −2.89 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
Zr1	0.34664 (4)	0.2500	0.19076 (5)	0.00788 (14)
Zr2	0.37045 (4)	0.2500	0.47072 (5)	0.00721 (13)
Zr3	0.39237 (4)	0.2500	0.90990 (5)	0.00782 (14)
Ni1	0.43680 (5)	0.2500	0.68908 (6)	0.00903 (18)
Sb1	0.02147 (3)	0.2500	0.29766 (3)	0.00871 (11)
Sb2	0.03748 (2)	0.2500	0.07626 (3)	0.00790 (10)
Sb3	0.07123 (3)	0.2500	0.56057 (3)	0.00957 (11)
Sb4	0.09131 (3)	0.2500	0.82504 (3)	0.00823 (10)
Sb5	0.22833 (3)	0.2500	0.35390 (3)	0.00918 (11)
Sb6	0.24792 (2)	0.2500	0.02153 (3)	0.00875 (11)
Sb7	0.28995 (3)	0.2500	0.68532 (4)	0.01218 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zr1	0.0068 (3)	0.0083 (3)	0.0085 (3)	0.000	−0.0007 (2)	0.000
Zr2	0.0054 (3)	0.0077 (3)	0.0085 (3)	0.000	0.0002 (2)	0.000
Zr3	0.0064 (3)	0.0078 (3)	0.0092 (3)	0.000	0.0004 (2)	0.000
Ni1	0.0085 (4)	0.0092 (5)	0.0094 (4)	0.000	0.0000 (3)	0.000
Sb1	0.0081 (2)	0.0089 (2)	0.0092 (2)	0.000	−0.00158 (15)	0.000
Sb2	0.0069 (2)	0.0084 (2)	0.0084 (2)	0.000	0.00046 (15)	0.000
Sb3	0.0104 (2)	0.0100 (2)	0.0083 (2)	0.000	0.00042 (16)	0.000
Sb4	0.0082 (2)	0.0086 (2)	0.0079 (2)	0.000	0.00022 (15)	0.000
Sb5	0.0069 (2)	0.0104 (2)	0.0102 (2)	0.000	0.00005 (15)	0.000
Sb6	0.0069 (2)	0.0100 (2)	0.0094 (2)	0.000	−0.00051 (15)	0.000
Sb7	0.0076 (2)	0.0100 (3)	0.0189 (3)	0.000	0.00142 (16)	0.000

Geometric parameters (Å, º) top

Zr1—Sb4ⁱ	2.9620 (6)	Sb2—Ni1ⁱⁱ	2.5876 (7)
Zr1—Sb4ⁱⁱ	2.9620 (6)	Sb2—Zr2ⁱⁱ	2.9604 (6)
Zr1—Sb6	2.9876 (8)	Sb2—Zr2ⁱ	2.9604 (6)
Zr1—Sb1ⁱⁱⁱ	3.0669 (8)	Sb2—Zr2^viii	3.0030 (8)
Zr1—Sb3ⁱⁱ	3.0720 (7)	Sb2—Sb2^xi	3.2250 (7)
Zr1—Sb3ⁱ	3.0720 (7)	Sb2—Sb2^xii	3.2250 (7)
Zr1—Sb7ⁱⁱ	3.0960 (6)	Sb2—Sb4^x	3.3111 (6)
Zr1—Sb7ⁱ	3.0960 (6)	Sb2—Sb4^ix	3.3111 (6)
Zr1—Sb5	3.1324 (8)	Sb3—Zr3ⁱⁱ	2.9943 (7)
Zr2—Sb6^iv	2.9478 (6)	Sb3—Zr3ⁱ	2.9943 (7)
Zr2—Sb6^v	2.9478 (6)	Sb3—Zr1^v	3.0720 (7)
Zr2—Sb4ⁱⁱ	2.9499 (6)	Sb3—Zr1^iv	3.0720 (7)
Zr2—Sb4ⁱ	2.9499 (6)	Sb3—Zr3^xiii	3.1617 (9)
Zr2—Sb2^v	2.9604 (6)	Sb3—Sb1^ix	3.2645 (6)
Zr2—Sb2^iv	2.9604 (6)	Sb3—Sb1^x	3.2645 (6)
Zr2—Sb2ⁱⁱⁱ	3.0029 (8)	Sb4—Ni1^xiii	2.7141 (10)
Zr2—Sb5	3.0044 (8)	Sb4—Zr2^v	2.9499 (6)
Zr2—Sb7	3.3962 (9)	Sb4—Zr2^iv	2.9499 (6)
Zr3—Sb1^iv	2.9569 (6)	Sb4—Zr1^iv	2.9619 (6)
Zr3—Sb1^v	2.9569 (6)	Sb4—Zr1^v	2.9619 (6)
Zr3—Sb3^v	2.9944 (7)	Sb4—Sb1^x	3.2981 (6)
Zr3—Sb3^iv	2.9944 (7)	Sb4—Sb1^ix	3.2981 (6)
Zr3—Sb5^iv	2.9958 (6)	Sb4—Sb2^x	3.3111 (6)
Zr3—Sb5^v	2.9958 (6)	Sb4—Sb2^ix	3.3110 (6)
Zr3—Sb6^vi	2.9975 (8)	Sb5—Zr3ⁱⁱ	2.9958 (6)
Zr3—Sb3^vii	3.1616 (9)	Sb5—Zr3ⁱ	2.9958 (6)
Zr3—Ni1	3.2730 (12)	Sb5—Sb7ⁱⁱ	3.1380 (6)
Ni1—Sb7	2.5728 (10)	Sb5—Sb7ⁱ	3.1380 (6)
Ni1—Sb2^iv	2.5875 (7)	Sb5—Sb6^v	3.1387 (6)
Ni1—Sb2^v	2.5875 (7)	Sb5—Sb6^iv	3.1387 (6)
Ni1—Sb1^v	2.6140 (7)	Sb6—Zr2ⁱⁱ	2.9478 (6)
Ni1—Sb1^iv	2.6140 (7)	Sb6—Zr2ⁱ	2.9478 (6)
Ni1—Sb4^vii	2.7141 (10)	Sb6—Zr3^xiv	2.9974 (8)
Sb1—Ni1ⁱⁱ	2.6139 (7)	Sb6—Sb5ⁱⁱ	3.1388 (6)
Sb1—Ni1ⁱ	2.6139 (7)	Sb6—Sb5ⁱ	3.1388 (6)
Sb1—Zr3ⁱ	2.9570 (6)	Sb6—Sb7ⁱ	3.1393 (6)
Sb1—Zr3ⁱⁱ	2.9570 (6)	Sb6—Sb7ⁱⁱ	3.1393 (6)
Sb1—Zr1^viii	3.0669 (8)	Sb7—Zr1^iv	3.0960 (6)
Sb1—Sb2	3.1998 (8)	Sb7—Zr1^v	3.0960 (6)
Sb1—Sb3^ix	3.2645 (6)	Sb7—Sb5^v	3.1380 (6)
Sb1—Sb3^x	3.2645 (6)	Sb7—Sb5^iv	3.1380 (6)
Sb1—Sb4^x	3.2981 (6)	Sb7—Sb6^iv	3.1393 (6)
Sb1—Sb4^ix	3.2981 (6)	Sb7—Sb6^v	3.1393 (6)
Sb2—Ni1ⁱ	2.5876 (7)

Sb4ⁱ—Zr1—Sb4ⁱⁱ	83.03 (2)	Ni1ⁱ—Sb2—Zr2^viii	108.12 (2)
Sb4ⁱ—Zr1—Sb6	138.128 (11)	Ni1ⁱⁱ—Sb2—Zr2^viii	108.12 (2)
Sb4ⁱⁱ—Zr1—Sb6	138.128 (11)	Zr2ⁱⁱ—Sb2—Zr2^viii	114.528 (17)
Sb4ⁱ—Zr1—Sb1ⁱⁱⁱ	66.303 (16)	Zr2ⁱ—Sb2—Zr2^viii	114.528 (17)
Sb4ⁱⁱ—Zr1—Sb1ⁱⁱⁱ	66.303 (16)	Ni1ⁱ—Sb2—Sb1	52.409 (19)
Sb6—Zr1—Sb1ⁱⁱⁱ	128.48 (3)	Ni1ⁱⁱ—Sb2—Sb1	52.409 (19)
Sb4ⁱ—Zr1—Sb3ⁱⁱ	130.54 (3)	Zr2ⁱⁱ—Sb2—Sb1	123.991 (17)
Sb4ⁱⁱ—Zr1—Sb3ⁱⁱ	78.623 (15)	Zr2ⁱ—Sb2—Sb1	123.991 (17)
Sb6—Zr1—Sb3ⁱⁱ	76.910 (19)	Zr2^viii—Sb2—Sb1	97.986 (19)
Sb1ⁱⁱⁱ—Zr1—Sb3ⁱⁱ	64.250 (16)	Ni1ⁱ—Sb2—Sb2^xi	163.78 (3)
Sb4ⁱ—Zr1—Sb3ⁱ	78.623 (15)	Ni1ⁱⁱ—Sb2—Sb2^xi	92.085 (17)
Sb4ⁱⁱ—Zr1—Sb3ⁱ	130.54 (3)	Zr2ⁱⁱ—Sb2—Sb2^xi	57.900 (17)
Sb6—Zr1—Sb3ⁱ	76.911 (19)	Zr2ⁱ—Sb2—Sb2^xi	106.03 (2)
Sb1ⁱⁱⁱ—Zr1—Sb3ⁱ	64.250 (16)	Zr2^viii—Sb2—Sb2^xi	56.628 (16)
Sb3ⁱⁱ—Zr1—Sb3ⁱ	79.45 (2)	Sb1—Sb2—Sb2^xi	129.982 (17)
Sb4ⁱ—Zr1—Sb7ⁱⁱ	136.09 (3)	Ni1ⁱ—Sb2—Sb2^xii	92.085 (17)
Sb4ⁱⁱ—Zr1—Sb7ⁱⁱ	83.092 (15)	Ni1ⁱⁱ—Sb2—Sb2^xii	163.78 (3)
Sb6—Zr1—Sb7ⁱⁱ	62.103 (16)	Zr2ⁱⁱ—Sb2—Sb2^xii	106.03 (2)
Sb1ⁱⁱⁱ—Zr1—Sb7ⁱⁱ	140.627 (10)	Zr2ⁱ—Sb2—Sb2^xii	57.900 (16)
Sb3ⁱⁱ—Zr1—Sb7ⁱⁱ	86.630 (15)	Zr2^viii—Sb2—Sb2^xii	56.628 (16)
Sb3ⁱ—Zr1—Sb7ⁱⁱ	138.75 (3)	Sb1—Sb2—Sb2^xii	129.982 (17)
Sb4ⁱ—Zr1—Sb7ⁱ	83.092 (15)	Sb2^xi—Sb2—Sb2^xii	75.00 (2)
Sb4ⁱⁱ—Zr1—Sb7ⁱ	136.09 (3)	Ni1ⁱ—Sb2—Sb4^x	107.40 (3)
Sb6—Zr1—Sb7ⁱ	62.103 (16)	Ni1ⁱⁱ—Sb2—Sb4^x	53.08 (2)
Sb1ⁱⁱⁱ—Zr1—Sb7ⁱ	140.627 (10)	Zr2ⁱⁱ—Sb2—Sb4^x	101.431 (12)
Sb3ⁱⁱ—Zr1—Sb7ⁱ	138.75 (3)	Zr2ⁱ—Sb2—Sb4^x	169.95 (2)
Sb3ⁱ—Zr1—Sb7ⁱ	86.630 (15)	Zr2^viii—Sb2—Sb4^x	55.446 (14)
Sb7ⁱⁱ—Zr1—Sb7ⁱ	78.71 (2)	Sb1—Sb2—Sb4^x	60.840 (12)
Sb4ⁱ—Zr1—Sb5	75.722 (19)	Sb2^xi—Sb2—Sb4^x	69.745 (15)
Sb4ⁱⁱ—Zr1—Sb5	75.722 (19)	Sb2^xii—Sb2—Sb4^x	112.07 (2)
Sb6—Zr1—Sb5	103.21 (2)	Ni1ⁱ—Sb2—Sb4^ix	53.08 (2)
Sb1ⁱⁱⁱ—Zr1—Sb5	128.31 (3)	Ni1ⁱⁱ—Sb2—Sb4^ix	107.40 (3)
Sb3ⁱⁱ—Zr1—Sb5	140.115 (11)	Zr2ⁱⁱ—Sb2—Sb4^ix	169.95 (2)
Sb3ⁱ—Zr1—Sb5	140.115 (11)	Zr2ⁱ—Sb2—Sb4^ix	101.431 (12)
Sb7ⁱⁱ—Zr1—Sb5	60.504 (16)	Zr2^viii—Sb2—Sb4^ix	55.446 (14)
Sb7ⁱ—Zr1—Sb5	60.504 (16)	Sb1—Sb2—Sb4^ix	60.840 (12)
Sb6^iv—Zr2—Sb6^v	83.52 (2)	Sb2^xi—Sb2—Sb4^ix	112.07 (2)
Sb6^iv—Zr2—Sb4ⁱⁱ	83.851 (14)	Sb2^xii—Sb2—Sb4^ix	69.745 (15)
Sb6^v—Zr2—Sb4ⁱⁱ	141.21 (3)	Sb4^x—Sb2—Sb4^ix	72.732 (15)
Sb6^iv—Zr2—Sb4ⁱ	141.21 (3)	Zr3ⁱⁱ—Sb3—Zr3ⁱ	81.94 (2)
Sb6^v—Zr2—Sb4ⁱ	83.851 (14)	Zr3ⁱⁱ—Sb3—Zr1^v	139.58 (2)
Sb4ⁱⁱ—Zr2—Sb4ⁱ	83.45 (2)	Zr3ⁱ—Sb3—Zr1^v	85.597 (17)
Sb6^iv—Zr2—Sb2^v	134.23 (3)	Zr3ⁱⁱ—Sb3—Zr1^iv	85.597 (16)
Sb6^v—Zr2—Sb2^v	79.287 (15)	Zr3ⁱ—Sb3—Zr1^iv	139.58 (2)
Sb4ⁱⁱ—Zr2—Sb2^v	133.05 (3)	Zr1^v—Sb3—Zr1^iv	79.45 (2)
Sb4ⁱ—Zr2—Sb2^v	78.456 (15)	Zr3ⁱⁱ—Sb3—Zr3^xiii	107.962 (18)
Sb6^iv—Zr2—Sb2^iv	79.287 (15)	Zr3ⁱ—Sb3—Zr3^xiii	107.962 (18)
Sb6^v—Zr2—Sb2^iv	134.23 (3)	Zr1^v—Sb3—Zr3^xiii	112.458 (19)
Sb4ⁱⁱ—Zr2—Sb2^iv	78.456 (15)	Zr1^iv—Sb3—Zr3^xiii	112.458 (19)
Sb4ⁱ—Zr2—Sb2^iv	133.05 (3)	Zr3ⁱⁱ—Sb3—Sb1^ix	162.39 (2)
Sb2^v—Zr2—Sb2^iv	83.09 (2)	Zr3ⁱ—Sb3—Sb1^ix	99.468 (13)
Sb6^iv—Zr2—Sb2ⁱⁱⁱ	137.839 (11)	Zr1^v—Sb3—Sb1^ix	57.799 (16)
Sb6^v—Zr2—Sb2ⁱⁱⁱ	137.839 (11)	Zr1^iv—Sb3—Sb1^ix	103.64 (2)
Sb4ⁱⁱ—Zr2—Sb2ⁱⁱⁱ	67.583 (16)	Zr3^xiii—Sb3—Sb1^ix	54.764 (13)
Sb4ⁱ—Zr2—Sb2ⁱⁱⁱ	67.583 (16)	Zr3ⁱⁱ—Sb3—Sb1^x	99.468 (13)
Sb2^v—Zr2—Sb2ⁱⁱⁱ	65.474 (17)	Zr3ⁱ—Sb3—Sb1^x	162.39 (2)
Sb2^iv—Zr2—Sb2ⁱⁱⁱ	65.474 (17)	Zr1^v—Sb3—Sb1^x	103.64 (2)
Sb6^iv—Zr2—Sb5	63.641 (17)	Zr1^iv—Sb3—Sb1^x	57.799 (15)
Sb6^v—Zr2—Sb5	63.641 (17)	Zr3^xiii—Sb3—Sb1^x	54.764 (13)
Sb4ⁱⁱ—Zr2—Sb5	77.886 (19)	Sb1^ix—Sb3—Sb1^x	73.942 (15)
Sb4ⁱ—Zr2—Sb5	77.886 (19)	Ni1^xiii—Sb4—Zr2^v	106.24 (2)
Sb2^v—Zr2—Sb5	137.621 (11)	Ni1^xiii—Sb4—Zr2^iv	106.24 (2)
Sb2^iv—Zr2—Sb5	137.621 (12)	Zr2^v—Sb4—Zr2^iv	83.45 (2)
Sb2ⁱⁱⁱ—Zr2—Sb5	132.94 (3)	Ni1^xiii—Sb4—Zr1^iv	108.49 (2)
Sb6^iv—Zr2—Sb7	58.813 (15)	Zr2^v—Sb4—Zr1^iv	145.27 (2)
Sb6^v—Zr2—Sb7	58.813 (15)	Zr2^iv—Sb4—Zr1^iv	86.535 (17)
Sb4ⁱⁱ—Zr2—Sb7	137.823 (12)	Ni1^xiii—Sb4—Zr1^v	108.49 (2)
Sb4ⁱ—Zr2—Sb7	137.823 (12)	Zr2^v—Sb4—Zr1^v	86.535 (17)
Sb2^v—Zr2—Sb7	76.068 (18)	Zr2^iv—Sb4—Zr1^v	145.27 (2)
Sb2^iv—Zr2—Sb7	76.068 (18)	Zr1^iv—Sb4—Zr1^v	83.03 (2)
Sb2ⁱⁱⁱ—Zr2—Sb7	127.55 (2)	Ni1^xiii—Sb4—Sb1^x	50.403 (16)
Sb5—Zr2—Sb7	99.51 (2)	Zr2^v—Sb4—Sb1^x	155.92 (2)
Sb1^iv—Zr3—Sb1^v	83.21 (2)	Zr2^iv—Sb4—Sb1^x	96.928 (13)
Sb1^iv—Zr3—Sb3^v	136.27 (3)	Zr1^iv—Sb4—Sb1^x	58.375 (16)
Sb1^v—Zr3—Sb3^v	81.481 (15)	Zr1^v—Sb4—Sb1^x	105.36 (2)
Sb1^iv—Zr3—Sb3^iv	81.481 (16)	Ni1^xiii—Sb4—Sb1^ix	50.403 (16)
Sb1^v—Zr3—Sb3^iv	136.27 (3)	Zr2^v—Sb4—Sb1^ix	96.928 (13)
Sb3^v—Zr3—Sb3^iv	81.94 (2)	Zr2^iv—Sb4—Sb1^ix	155.92 (2)
Sb1^iv—Zr3—Sb5^iv	77.172 (16)	Zr1^iv—Sb4—Sb1^ix	105.36 (2)
Sb1^v—Zr3—Sb5^iv	130.41 (3)	Zr1^v—Sb4—Sb1^ix	58.375 (16)
Sb3^v—Zr3—Sb5^iv	140.80 (3)	Sb1^x—Sb4—Sb1^ix	73.066 (15)
Sb3^iv—Zr3—Sb5^iv	85.155 (14)	Ni1^xiii—Sb4—Sb2^x	49.662 (16)
Sb1^iv—Zr3—Sb5^v	130.41 (3)	Zr2^v—Sb4—Sb2^x	104.14 (2)
Sb1^v—Zr3—Sb5^v	77.172 (15)	Zr2^iv—Sb4—Sb2^x	56.972 (16)
Sb3^v—Zr3—Sb5^v	85.155 (14)	Zr1^iv—Sb4—Sb2^x	97.880 (13)
Sb3^iv—Zr3—Sb5^v	140.80 (3)	Zr1^v—Sb4—Sb2^x	157.39 (2)
Sb5^iv—Zr3—Sb5^v	81.89 (2)	Sb1^x—Sb4—Sb2^x	57.912 (14)
Sb1^iv—Zr3—Sb6^vi	136.371 (13)	Sb1^ix—Sb4—Sb2^x	100.063 (17)
Sb1^v—Zr3—Sb6^vi	136.371 (13)	Ni1^xiii—Sb4—Sb2^ix	49.662 (16)
Sb3^v—Zr3—Sb6^vi	77.956 (19)	Zr2^v—Sb4—Sb2^ix	56.972 (16)
Sb3^iv—Zr3—Sb6^vi	77.956 (19)	Zr2^iv—Sb4—Sb2^ix	104.14 (2)
Sb5^iv—Zr3—Sb6^vi	63.164 (17)	Zr1^iv—Sb4—Sb2^ix	157.39 (2)
Sb5^v—Zr3—Sb6^vi	63.164 (17)	Zr1^v—Sb4—Sb2^ix	97.880 (13)
Sb1^iv—Zr3—Sb3^vii	64.388 (16)	Sb1^x—Sb4—Sb2^ix	100.063 (17)
Sb1^v—Zr3—Sb3^vii	64.388 (16)	Sb1^ix—Sb4—Sb2^ix	57.912 (14)
Sb3^v—Zr3—Sb3^vii	72.038 (18)	Sb2^x—Sb4—Sb2^ix	72.734 (15)
Sb3^iv—Zr3—Sb3^vii	72.038 (18)	Zr3ⁱⁱ—Sb5—Zr3ⁱ	81.89 (2)
Sb5^iv—Zr3—Sb3^vii	137.351 (12)	Zr3ⁱⁱ—Sb5—Zr2	115.73 (2)
Sb5^v—Zr3—Sb3^vii	137.351 (12)	Zr3ⁱ—Sb5—Zr2	115.73 (2)
Sb6^vi—Zr3—Sb3^vii	139.85 (3)	Zr3ⁱⁱ—Sb5—Zr1	131.970 (16)
Sb1^iv—Zr3—Ni1	49.295 (15)	Zr3ⁱ—Sb5—Zr1	131.970 (16)
Sb1^v—Zr3—Ni1	49.295 (15)	Zr2—Sb5—Zr1	82.62 (2)
Sb3^v—Zr3—Ni1	130.769 (18)	Zr3ⁱⁱ—Sb5—Sb7ⁱⁱ	74.105 (16)
Sb3^iv—Zr3—Ni1	130.769 (18)	Zr3ⁱ—Sb5—Sb7ⁱⁱ	123.11 (2)
Sb5^iv—Zr3—Ni1	84.63 (2)	Zr2—Sb5—Sb7ⁱⁱ	121.163 (17)
Sb5^v—Zr3—Ni1	84.63 (2)	Zr1—Sb5—Sb7ⁱⁱ	59.174 (15)
Sb6^vi—Zr3—Ni1	136.18 (3)	Zr3ⁱⁱ—Sb5—Sb7ⁱ	123.11 (2)
Sb3^vii—Zr3—Ni1	83.97 (2)	Zr3ⁱ—Sb5—Sb7ⁱ	74.105 (16)
Sb7—Ni1—Sb2^iv	99.26 (3)	Zr2—Sb5—Sb7ⁱ	121.163 (17)
Sb7—Ni1—Sb2^v	99.26 (3)	Zr1—Sb5—Sb7ⁱ	59.174 (15)
Sb2^iv—Ni1—Sb2^v	98.71 (3)	Sb7ⁱⁱ—Sb5—Sb7ⁱ	77.460 (18)
Sb7—Ni1—Sb1^v	106.99 (3)	Zr3ⁱⁱ—Sb5—Sb6^v	107.25 (2)
Sb2^iv—Ni1—Sb1^v	153.71 (4)	Zr3ⁱ—Sb5—Sb6^v	58.444 (16)
Sb2^v—Ni1—Sb1^v	75.925 (16)	Zr2—Sb5—Sb6^v	57.301 (14)
Sb7—Ni1—Sb1^iv	106.99 (3)	Zr1—Sb5—Sb6^v	119.266 (16)
Sb2^iv—Ni1—Sb1^iv	75.925 (16)	Sb7ⁱⁱ—Sb5—Sb6^v	178.23 (2)
Sb2^v—Ni1—Sb1^iv	153.71 (4)	Sb7ⁱ—Sb5—Sb6^v	102.523 (11)
Sb1^v—Ni1—Sb1^iv	97.37 (3)	Zr3ⁱⁱ—Sb5—Sb6^iv	58.444 (16)
Sb7—Ni1—Sb4^vii	174.50 (4)	Zr3ⁱ—Sb5—Sb6^iv	107.25 (2)
Sb2^iv—Ni1—Sb4^vii	77.26 (2)	Zr2—Sb5—Sb6^iv	57.302 (14)
Sb2^v—Ni1—Sb4^vii	77.26 (2)	Zr1—Sb5—Sb6^iv	119.266 (16)
Sb1^v—Ni1—Sb4^vii	76.46 (2)	Sb7ⁱⁱ—Sb5—Sb6^iv	102.523 (11)
Sb1^iv—Ni1—Sb4^vii	76.46 (2)	Sb7ⁱ—Sb5—Sb6^iv	178.23 (2)
Sb7—Ni1—Zr3	77.45 (3)	Sb6^v—Sb5—Sb6^iv	77.438 (18)
Sb2^iv—Ni1—Zr3	130.623 (17)	Zr2ⁱⁱ—Sb6—Zr2ⁱ	83.52 (2)
Sb2^v—Ni1—Zr3	130.623 (17)	Zr2ⁱⁱ—Sb6—Zr1	127.554 (17)
Sb1^v—Ni1—Zr3	59.04 (2)	Zr2ⁱ—Sb6—Zr1	127.554 (17)
Sb1^iv—Ni1—Zr3	59.04 (2)	Zr2ⁱⁱ—Sb6—Zr3^xiv	117.435 (19)
Sb4^vii—Ni1—Zr3	108.05 (3)	Zr2ⁱ—Sb6—Zr3^xiv	117.435 (19)
Ni1ⁱⁱ—Sb1—Ni1ⁱ	97.37 (3)	Zr1—Sb6—Zr3^xiv	87.06 (2)
Ni1ⁱⁱ—Sb1—Zr3ⁱ	133.06 (3)	Zr2ⁱⁱ—Sb6—Sb5ⁱⁱ	59.058 (16)
Ni1ⁱ—Sb1—Zr3ⁱ	71.66 (2)	Zr2ⁱ—Sb6—Sb5ⁱⁱ	108.60 (2)
Ni1ⁱⁱ—Sb1—Zr3ⁱⁱ	71.66 (2)	Zr1—Sb6—Sb5ⁱⁱ	123.387 (17)
Ni1ⁱ—Sb1—Zr3ⁱⁱ	133.06 (3)	Zr3^xiv—Sb6—Sb5ⁱⁱ	58.391 (14)
Zr3ⁱ—Sb1—Zr3ⁱⁱ	83.21 (2)	Zr2ⁱⁱ—Sb6—Sb5ⁱ	108.60 (2)
Ni1ⁱⁱ—Sb1—Zr1^viii	108.17 (2)	Zr2ⁱ—Sb6—Sb5ⁱ	59.058 (16)
Ni1ⁱ—Sb1—Zr1^viii	108.17 (2)	Zr1—Sb6—Sb5ⁱ	123.387 (17)
Zr3ⁱ—Sb1—Zr1^viii	118.681 (19)	Zr3^xiv—Sb6—Sb5ⁱ	58.391 (14)
Zr3ⁱⁱ—Sb1—Zr1^viii	118.681 (19)	Sb5ⁱⁱ—Sb6—Sb5ⁱ	77.437 (18)
Ni1ⁱⁱ—Sb1—Sb2	51.665 (19)	Zr2ⁱⁱ—Sb6—Sb7ⁱ	117.02 (2)
Ni1ⁱ—Sb1—Sb2	51.665 (19)	Zr2ⁱ—Sb6—Sb7ⁱ	67.743 (16)
Zr3ⁱ—Sb1—Sb2	119.976 (18)	Zr1—Sb6—Sb7ⁱ	60.643 (16)
Zr3ⁱⁱ—Sb1—Sb2	119.976 (18)	Zr3^xiv—Sb6—Sb7ⁱ	125.528 (15)
Zr1^viii—Sb1—Sb2	98.147 (19)	Sb5ⁱⁱ—Sb6—Sb7ⁱ	175.37 (2)
Ni1ⁱⁱ—Sb1—Sb3^ix	164.74 (2)	Sb5ⁱ—Sb6—Sb7ⁱ	102.379 (11)
Ni1ⁱ—Sb1—Sb3^ix	93.514 (18)	Zr2ⁱⁱ—Sb6—Sb7ⁱⁱ	67.743 (16)
Zr3ⁱ—Sb1—Sb3^ix	60.848 (17)	Zr2ⁱ—Sb6—Sb7ⁱⁱ	117.02 (2)
Zr3ⁱⁱ—Sb1—Sb3^ix	108.15 (2)	Zr1—Sb6—Sb7ⁱⁱ	60.643 (16)
Zr1^viii—Sb1—Sb3^ix	57.951 (14)	Zr3^xiv—Sb6—Sb7ⁱⁱ	125.528 (15)
Sb2—Sb1—Sb3^ix	131.792 (14)	Sb5ⁱⁱ—Sb6—Sb7ⁱⁱ	102.379 (11)
Ni1ⁱⁱ—Sb1—Sb3^x	93.514 (18)	Sb5ⁱ—Sb6—Sb7ⁱⁱ	175.37 (2)
Ni1ⁱ—Sb1—Sb3^x	164.74 (2)	Sb7ⁱ—Sb6—Sb7ⁱⁱ	77.422 (18)
Zr3ⁱ—Sb1—Sb3^x	108.15 (2)	Ni1—Sb7—Zr1^iv	140.543 (10)
Zr3ⁱⁱ—Sb1—Sb3^x	60.848 (17)	Ni1—Sb7—Zr1^v	140.543 (10)
Zr1^viii—Sb1—Sb3^x	57.951 (14)	Zr1^iv—Sb7—Zr1^v	78.71 (2)
Sb2—Sb1—Sb3^x	131.792 (13)	Ni1—Sb7—Sb5^v	94.92 (2)
Sb3^ix—Sb1—Sb3^x	73.942 (16)	Zr1^iv—Sb7—Sb5^v	107.36 (2)
Ni1ⁱⁱ—Sb1—Sb4^x	53.14 (2)	Zr1^v—Sb7—Sb5^v	60.321 (16)
Ni1ⁱ—Sb1—Sb4^x	107.12 (3)	Ni1—Sb7—Sb5^iv	94.92 (2)
Zr3ⁱ—Sb1—Sb4^x	173.544 (17)	Zr1^iv—Sb7—Sb5^iv	60.321 (16)
Zr3ⁱⁱ—Sb1—Sb4^x	101.722 (12)	Zr1^v—Sb7—Sb5^iv	107.36 (2)
Zr1^viii—Sb1—Sb4^x	55.321 (14)	Sb5^v—Sb7—Sb5^iv	77.460 (18)
Sb2—Sb1—Sb4^x	61.249 (13)	Ni1—Sb7—Sb6^iv	103.12 (2)
Sb3^ix—Sb1—Sb4^x	113.263 (18)	Zr1^iv—Sb7—Sb6^iv	57.253 (16)
Sb3^x—Sb1—Sb4^x	71.272 (14)	Zr1^v—Sb7—Sb6^iv	104.61 (2)
Ni1ⁱⁱ—Sb1—Sb4^ix	107.12 (3)	Sb5^v—Sb7—Sb6^iv	161.93 (2)
Ni1ⁱ—Sb1—Sb4^ix	53.14 (2)	Sb5^iv—Sb7—Sb6^iv	99.677 (12)
Zr3ⁱ—Sb1—Sb4^ix	101.722 (12)	Ni1—Sb7—Sb6^v	103.12 (2)
Zr3ⁱⁱ—Sb1—Sb4^ix	173.544 (17)	Zr1^iv—Sb7—Sb6^v	104.61 (2)
Zr1^viii—Sb1—Sb4^ix	55.321 (14)	Zr1^v—Sb7—Sb6^v	57.253 (16)
Sb2—Sb1—Sb4^ix	61.249 (13)	Sb5^v—Sb7—Sb6^v	99.677 (12)
Sb3^ix—Sb1—Sb4^ix	71.272 (14)	Sb5^iv—Sb7—Sb6^v	161.93 (2)
Sb3^x—Sb1—Sb4^ix	113.263 (18)	Sb6^iv—Sb7—Sb6^v	77.422 (18)
Sb4^x—Sb1—Sb4^ix	73.066 (15)	Ni1—Sb7—Zr2	66.67 (2)
Ni1ⁱ—Sb2—Ni1ⁱⁱ	98.71 (3)	Zr1^iv—Sb7—Zr2	110.11 (2)
Ni1ⁱ—Sb2—Zr2ⁱⁱ	136.93 (3)	Zr1^v—Sb7—Zr2	110.11 (2)
Ni1ⁱⁱ—Sb2—Zr2ⁱⁱ	73.99 (2)	Sb5^v—Sb7—Zr2	138.240 (11)
Ni1ⁱ—Sb2—Zr2ⁱ	73.99 (2)	Sb5^iv—Sb7—Zr2	138.240 (11)
Ni1ⁱⁱ—Sb2—Zr2ⁱ	136.93 (3)	Sb6^iv—Sb7—Zr2	53.446 (14)
Zr2ⁱⁱ—Sb2—Zr2ⁱ	83.09 (2)	Sb6^v—Sb7—Zr2	53.446 (14)

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

Experimental details

Crystal data
Chemical formula	Zr₃NiSb₇
M_r	1184.62
Crystal system, space group	Orthorhombic, Pnma
Temperature (K)	295
a, b, c (Å)	17.5165 (19), 3.9266 (4), 14.3968 (15)
V (Å³)	990.22 (18)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	23.56
Crystal size (mm)	0.37 × 0.06 × 0.04

Data collection
Diffractometer	Bruker SMART 1000 diffractometer
Absorption correction	Numerical (SHELXTL; Sheldrick, 2008)
T_min, T_max	0.057, 0.426
No. of measured, independent and observed [I > 2σ(I)] reflections	11118, 1722, 1500
R_int	0.044
(sin θ/λ)_max (Å⁻¹)	0.714

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.054, 1.18
No. of reflections	1722
No. of parameters	68
Δρ_max, Δρ_min (e Å⁻³)	2.12, −2.89

Computer programs: SMART (Bruker, 2000), SAINT-Plus (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999).

Selected bond lengths (Å) top

Zr1—Sb4ⁱ	2.9620 (6)	Zr3—Sb6^v	2.9975 (8)
Zr1—Sb6	2.9876 (8)	Zr3—Sb3^vi	3.1616 (9)
Zr1—Sb1ⁱⁱ	3.0669 (8)	Ni1—Sb7	2.5728 (10)
Zr1—Sb3ⁱⁱⁱ	3.0720 (7)	Ni1—Sb2^iv	2.5875 (7)
Zr1—Sb7ⁱⁱⁱ	3.0960 (6)	Ni1—Sb1^iv	2.6140 (7)
Zr1—Sb5	3.1324 (8)	Ni1—Sb4^vi	2.7141 (10)
Zr2—Sb6^iv	2.9478 (6)	Sb1—Sb2	3.1998 (8)
Zr2—Sb4ⁱⁱⁱ	2.9499 (6)	Sb1—Sb3^vii	3.2645 (6)
Zr2—Sb2^iv	2.9604 (6)	Sb1—Sb4^viii	3.2981 (6)
Zr2—Sb2ⁱⁱ	3.0029 (8)	Sb2—Sb2^ix	3.2250 (7)
Zr2—Sb5	3.0044 (8)	Sb2—Sb4^viii	3.3111 (6)
Zr3—Sb1^iv	2.9569 (6)	Sb5—Sb7ⁱⁱⁱ	3.1380 (6)
Zr3—Sb3^iv	2.9944 (7)	Sb5—Sb6^iv	3.1387 (6)
Zr3—Sb5^iv	2.9958 (6)	Sb6—Sb7ⁱ	3.1393 (6)

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

Acknowledgements

The work was in part supported by the Ministry of Ukraine for Education and Science (grant No. 0106U001299).

References

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