inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

TbNb6Sn6: the first ternary compound from the rare earth–niobium–tin system

aDepartment of Inorganic Chemistry, Ivan Franko Lviv National University, Kyryla and Mefodiya str. 6, 79005 Lviv, Ukraine, and bDepartment Chemie, Technische Universität München, Lichtenbergstr. 4, 85747 Garching, Germany
*Correspondence e-mail: romaniuk@ua.fm

(Received 26 October 2010; accepted 8 November 2010; online 17 November 2010)

The title compound, terbium hexa­niobium hexastannide, TbNb6Sn6, is the first ternary compound from the rare earth–niobium–tin system. It has the HfFe6Ge6 structure type, which can be analysed as an inter­growth of the Zr4Al3 and CaCu5 structures. All the atoms lie on special positions; their coordination geometries and site symmetries are: Tb (dodeca­hedron) 6/mmm; Nb (distorted icosa­hedron) 2mm; Sn (Frank–Caspar polyhedron, CN = 14–15) 6mm and [\overline{6}]m2; Sn (distorted icosa­hedron) [\overline{6}]m2. The structure contains a graphite-type Sn network, Kagome nets of Nb atoms, and Tb atoms alternating with Sn2 dumbbells in the channels.

Related literature

For background to niobium alloys, see: Ateev & Shamrai (1966[Ateev, N. V. & Shamrai, V. F. (1966). Inorg. Mater. (USSR), 2, 886-892.]). For related structures and background to inter­metallics, see: Nowotny (1942[Nowotny, H. (1942). Z. Metallkd. 34, 247-253.]); Raeuchle & Rundle (1952[Raeuchle, R. F. & Rundle, R. E. (1952). Acta Cryst. 5, 85-93.]); Schobinger-Papamantellos et al. (1998[Schobinger-Papamantellos, P., Buschow, K. H. J., de Boer, F. R., Ritter, C., Isnard, O. & Fauth, F. (1998). J. Alloys Compd, 267, 59-65.]); Wilson et al. (1960[Wilson, C. G., Thomas, D. K. & Spooner, F. J. (1960). Acta Cryst. 13, 56-57.]). A statistical test of the distribution of the E values using the program E-STATS from WinGX system (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]) suggested that the structure is centrosymmetric. For MgCo6Ge6, see: Gieck et al. (2006[Gieck, C., Schreyer, M., Fässler, T. F., Cavet, S. & Claus, P. (2006). Chem. Eur. J. 12, 1924-1930.]).

Experimental

Crystal data
  • TbNb6Sn6

  • Mr = 1428.52

  • Hexagonal, P 6/m m m

  • a = 5.7650 (1) Å

  • c = 9.5387 (4) Å

  • V = 274.55 (1) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 25.66 mm−1

  • T = 293 K

  • 0.050 × 0.020 × 0.004 mm

Data collection
  • Oxford Diffraction Xcalibur3 diffractometer with CCD detector

  • Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCDand CrysAlis RED. Oxford Diffraction, Yarnton, England.]) Tmin = 0.592, Tmax = 1.000

  • 2493 measured reflections

  • 208 independent reflections

  • 181 reflections with I > 2σ(I)

  • Rint = 0.027

Refinement
  • R[F2 > 2σ(F2)] = 0.017

  • wR(F2) = 0.038

  • S = 1.29

  • 208 reflections

  • 15 parameters

  • Δρmax = 1.68 e Å−3

  • Δρmin = −2.35 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCDand CrysAlis RED. Oxford Diffraction, Yarnton, England.]); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCDand CrysAlis RED. Oxford Diffraction, Yarnton, England.]); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

Niobium compounds have very useful properties for superconductive materials: high critical fields and plasticity which gives an opportunity to make superconductive windings. The main disadvantage of these compounds is the low critical temperature (Ateev & Shamrai, 1966). Superconductive Nb3Sn with Tc=18.2 K is a high performance superconductor and the gold standard of the world's superconductor industry.

So far, no ternary compounds in the RE–Nb–Sn (RE - rare-earth metals) systems are known. TbNb6Sn6 is the first ternary Rare earth – Niobium – Tin compound. According to the X-ray single-crystal data the TbNb6Sn6 compound crystallizes with hexagonal symmetry (space group P6/mmm, HfFe6Ge6 structure type). In TbNb6Sn6 planar graphite-type layers of Sn atoms and Kagome nets of Nb atoms alternate along the c axis, similar to the recently reported MgCo6Ge6 compound (Gieck et al., 2006). The resulting columns of vertex-sharing trigonal bipyramids form a three-dimensional Nb–Sn network with hexagonal tunnels (Figure 1). These tunnels are alternately centered by Tb atoms and Sn2 dumbbells (with Sn-Sn distances of 3.24 A). The coordination polyhedra of the atoms are: Tb1 — 20-vertex polyhedron (CN=20), Sn2 — Frank-Casper polyhedron (CN=15), Sn3 — distorted icosahedron (CN=12), Sn4 — Frank-Casper polyhedron (CN=14) and Nb5 — distorted icosahedron (CN=12).

The HfFe6Ge6 structure type (Schobinger-Papamantellos et al.,1998), also referred to MgFe6Ge6 or LiCo6Ge6, can be described as an intergrowth of the Zr4Al3 (Wilson et al., 1960) and CaCu5 (Nowotny, 1942) structure types (see Fig.2). Another possibility to describe the HfFe6Ge6 structure is a transformation of the CaCu5 structure via multiple substitution and ordering of atoms. The first step is the doubling of the CaCu5 unit cell along the c axis. The substitution of every second Ca atom (R) along the c axis by a pair of atoms (2X) transforms this structure into the hexagonal modification of TiBe12 (Raeuchle & Rundle, 1952). As a result, the c/a ratio increases to 1.733. Further ordering of X atoms in the TiBe12 leads to the HfFe6Ge6 structure. Perhaps the presence of atoms of different radii leads to closer packing of the layers in the ternary HfFe6Ge6 compared to the binary TiBe12. Therefore, the c/a ratio of 1.591 for ternary HfFe6Ge6 is much closer to the ideal value of 1.596 (c/a = 1.6546 for TbNb6Sn6).

Related literature top

For background to niobium alloys, see: Ateev & Shamrai (1966). For related structures and background to intermetallics, see: Nowotny (1942); Raeuchle & Rundle (1952); Schobinger-Papamantellos et al. (1998); Wilson et al. (1960). A statistical test of the distribution of the E values using the program E-STATS from WinGX system (Farrugia, 1999) suggested that the structure is centrosymmetric.

Experimental top

Single crystals of the title compound were first found in a sample with the composition 2Tb:3Zn:5Sn, which was synthesized by induction heating of the pure elements in a niobium crucible. The sample was heated at 1100° C in an induction furnace (Hüttinger Elektronik, Freiburg, Type TIG 2.5/300) under continuous argon flow for 1 h followed by cooling to 700° C at a rate of 10 degrees/min. Finally it was quenched by switching off the furnace. A reaction between the sample and the Nb container was observed. Good-quality hexagonal plate-like crystals were selected from annealed sample by mechanical fragmentation. Single-crystal intensity data of TbNb6Sn6 were collected at room temperature on an Oxford-Xcalibur3 CCD area detector diffractometer. After the measurement, the single crystal was analyzed with a JEOL SEM 5900LV scanning electron microscope. No impurity elements heavier than sodium were observed. The EDX analysis of well-shaped single crystal reveals the composition (in atomic percentages) Tb 8(3), Nb 45 (6), and Sn 47 (7), which is in good agreement with the compositions resulting from XRD data refinement. Further, a sample with the composition of Tb:6Nb:6Sn was prepared by arc melting and examined by powder X-ray diffraction. As-cast sample does not contain TbNb6Sn6 phase. However, after grinding, pressing and annealing it at 900°C for 12 h a significant amount of the TbNb6Sn6 phase was observed. Magnetic measurements of the annealed sample were performed using a MPMS XL5 SQUID magnetometer (Quantum Design). Cooling the sample without magnetic field and rising the temperature in the presence of a field of 15 Oe from 1.8 K to 50 K revealed at approximately 18 K only the superconducting behavior of the Nb3Sn impurity.

Refinement top

A statistical test of the distribution of the E values using the program E-STATS from WinGX system (Farrugia, 1999) suggested that the structure is centrosymmetric. The analysis of systematic extinctions yielded the space group P6/mmm, and it was confirmed by the following structure refinement. The structure was solved by the direct methods.

Structure description top

Niobium compounds have very useful properties for superconductive materials: high critical fields and plasticity which gives an opportunity to make superconductive windings. The main disadvantage of these compounds is the low critical temperature (Ateev & Shamrai, 1966). Superconductive Nb3Sn with Tc=18.2 K is a high performance superconductor and the gold standard of the world's superconductor industry.

So far, no ternary compounds in the RE–Nb–Sn (RE - rare-earth metals) systems are known. TbNb6Sn6 is the first ternary Rare earth – Niobium – Tin compound. According to the X-ray single-crystal data the TbNb6Sn6 compound crystallizes with hexagonal symmetry (space group P6/mmm, HfFe6Ge6 structure type). In TbNb6Sn6 planar graphite-type layers of Sn atoms and Kagome nets of Nb atoms alternate along the c axis, similar to the recently reported MgCo6Ge6 compound (Gieck et al., 2006). The resulting columns of vertex-sharing trigonal bipyramids form a three-dimensional Nb–Sn network with hexagonal tunnels (Figure 1). These tunnels are alternately centered by Tb atoms and Sn2 dumbbells (with Sn-Sn distances of 3.24 A). The coordination polyhedra of the atoms are: Tb1 — 20-vertex polyhedron (CN=20), Sn2 — Frank-Casper polyhedron (CN=15), Sn3 — distorted icosahedron (CN=12), Sn4 — Frank-Casper polyhedron (CN=14) and Nb5 — distorted icosahedron (CN=12).

The HfFe6Ge6 structure type (Schobinger-Papamantellos et al.,1998), also referred to MgFe6Ge6 or LiCo6Ge6, can be described as an intergrowth of the Zr4Al3 (Wilson et al., 1960) and CaCu5 (Nowotny, 1942) structure types (see Fig.2). Another possibility to describe the HfFe6Ge6 structure is a transformation of the CaCu5 structure via multiple substitution and ordering of atoms. The first step is the doubling of the CaCu5 unit cell along the c axis. The substitution of every second Ca atom (R) along the c axis by a pair of atoms (2X) transforms this structure into the hexagonal modification of TiBe12 (Raeuchle & Rundle, 1952). As a result, the c/a ratio increases to 1.733. Further ordering of X atoms in the TiBe12 leads to the HfFe6Ge6 structure. Perhaps the presence of atoms of different radii leads to closer packing of the layers in the ternary HfFe6Ge6 compared to the binary TiBe12. Therefore, the c/a ratio of 1.591 for ternary HfFe6Ge6 is much closer to the ideal value of 1.596 (c/a = 1.6546 for TbNb6Sn6).

For background to niobium alloys, see: Ateev & Shamrai (1966). For related structures and background to intermetallics, see: Nowotny (1942); Raeuchle & Rundle (1952); Schobinger-Papamantellos et al. (1998); Wilson et al. (1960). A statistical test of the distribution of the E values using the program E-STATS from WinGX system (Farrugia, 1999) suggested that the structure is centrosymmetric.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2008); cell refinement: CrysAlis CCD (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. View of the TbNb6Sn6 structure. The graphite-type Sn layers, Ge2 dumbbells and condensed Nb3Sn2 bipyramids are emphasized.
[Figure 2] Fig. 2. Relationships between the HfFe6Ge6, Zr4Al3 and CaCu5 structures.
terbium hexaniobium hexatin top
Crystal data top
TbNb6Sn6Dx = 8.640 Mg m3
Mr = 1428.52Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6/mmmCell parameters from 181 reflections
Hall symbol: -P 6 2θ = 4.1–30.0°
a = 5.7650 (1) ŵ = 25.66 mm1
c = 9.5387 (4) ÅT = 293 K
V = 274.55 (1) Å3Hexagonal plate, metallic gray
Z = 10.05 × 0.02 × 0.004 mm
F(000) = 611
Data collection top
Oxford Diffraction Xcalibur3
diffractometer with CCD detector
208 independent reflections
Radiation source: Enhance (Mo) X-ray Source181 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Detector resolution: 16.0238 pixels mm-1θmax = 30.0°, θmin = 4.1°
ω and π scansh = 87
Absorption correction: multi-scan
(CrysAlis RED, Oxford Diffraction, 2008)
k = 58
Tmin = 0.592, Tmax = 1.000l = 1313
2493 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017 w = 1/[σ2(Fo2) + (0.0113P)2 + 2.3749P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.038(Δ/σ)max < 0.001
S = 1.29Δρmax = 1.68 e Å3
208 reflectionsΔρmin = 2.35 e Å3
15 parametersExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0333 (12)
Crystal data top
TbNb6Sn6Z = 1
Mr = 1428.52Mo Kα radiation
Hexagonal, P6/mmmµ = 25.66 mm1
a = 5.7650 (1) ÅT = 293 K
c = 9.5387 (4) Å0.05 × 0.02 × 0.004 mm
V = 274.55 (1) Å3
Data collection top
Oxford Diffraction Xcalibur3
diffractometer with CCD detector
208 independent reflections
Absorption correction: multi-scan
(CrysAlis RED, Oxford Diffraction, 2008)
181 reflections with I > 2σ(I)
Tmin = 0.592, Tmax = 1.000Rint = 0.027
2493 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01715 parameters
wR(F2) = 0.0380 restraints
S = 1.29Δρmax = 1.68 e Å3
208 reflectionsΔρmin = 2.35 e Å3
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
xyzUiso*/Ueq
Tb10.00000.00000.00000.0101 (3)
Sn20.33330.66670.50000.0074 (2)
Sn30.33330.66670.00000.0066 (2)
Sn40.00000.00000.33003 (11)0.0091 (2)
Nb50.00000.50000.24932 (6)0.0053 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb10.0082 (3)0.0082 (3)0.0140 (5)0.00408 (16)0.0000.000
Sn20.0084 (3)0.0084 (3)0.0054 (4)0.00421 (14)0.0000.000
Sn30.0070 (3)0.0070 (3)0.0058 (4)0.00349 (14)0.0000.000
Sn40.0063 (3)0.0063 (3)0.0148 (5)0.00314 (15)0.0000.000
Nb50.0047 (3)0.0050 (3)0.0060 (3)0.00235 (17)0.0000.000
Geometric parameters (Å, º) top
Tb1—Sn43.1481 (10)Sn3—Nb5ix2.9027 (5)
Tb1—Sn4i3.1481 (10)Sn3—Nb52.9027 (5)
Tb1—Sn3ii3.3284Sn3—Tb1xiii3.3284
Tb1—Sn3iii3.3284Sn3—Tb1xiv3.3284
Tb1—Sn3i3.3284Sn4—Nb52.9835 (3)
Tb1—Sn33.3284Sn4—Nb5xv2.9835 (3)
Tb1—Sn3iv3.3285Sn4—Nb5ix2.9835 (3)
Tb1—Sn3v3.3285Sn4—Nb5xvi2.9835 (3)
Sn2—Nb52.9133 (5)Sn4—Nb5v2.9835 (3)
Sn2—Nb5vi2.9133 (5)Sn4—Nb5xvii2.9835 (3)
Sn2—Nb5vii2.9133 (5)Sn4—Sn4xviii3.243 (2)
Sn2—Nb5viii2.9133 (5)Nb5—Nb5viii2.8825
Sn2—Nb5ix2.9133 (5)Nb5—Nb5xvi2.8825
Sn2—Nb5x2.9133 (5)Nb5—Nb5ix2.8825
Sn3—Nb5viii2.9027 (5)Nb5—Nb5xix2.8825
Sn3—Nb5iv2.9027 (5)Nb5—Sn3iv2.9027 (5)
Sn3—Nb5xi2.9027 (5)Nb5—Sn2vii2.9133 (5)
Sn3—Nb5xii2.9027 (5)Nb5—Sn4xiii2.9835 (3)
Sn4—Tb1—Sn4i180.0Nb5—Sn3—Tb173.341 (3)
Sn4—Tb1—Sn3ii90.0Tb1xiii—Sn3—Tb1120.0
Sn4i—Tb1—Sn3ii90.0Tb1xiv—Sn3—Tb1120.0
Sn4—Tb1—Sn3iii90.0Nb5—Sn4—Nb5xv113.586 (17)
Sn4i—Tb1—Sn3iii90.0Nb5—Sn4—Nb5ix57.772 (6)
Sn3ii—Tb1—Sn3iii180.0Nb5xv—Sn4—Nb5ix150.09 (4)
Sn4—Tb1—Sn3i90.0Nb5—Sn4—Nb5xvi57.772 (6)
Sn4i—Tb1—Sn3i90.0Nb5xv—Sn4—Nb5xvi57.772 (6)
Sn3ii—Tb1—Sn3i120.0Nb5ix—Sn4—Nb5xvi113.586 (17)
Sn3iii—Tb1—Sn3i60.0Nb5—Sn4—Nb5v150.09 (4)
Sn4—Tb1—Sn390.0Nb5xv—Sn4—Nb5v57.772 (6)
Sn4i—Tb1—Sn390.0Nb5ix—Sn4—Nb5v113.586 (17)
Sn3ii—Tb1—Sn360.0Nb5xvi—Sn4—Nb5v113.586 (17)
Sn3iii—Tb1—Sn3120.0Nb5—Sn4—Nb5xvii113.586 (17)
Sn3i—Tb1—Sn3180.0Nb5xv—Sn4—Nb5xvii113.586 (17)
Sn4—Tb1—Sn3iv90.0Nb5ix—Sn4—Nb5xvii57.772 (6)
Sn4i—Tb1—Sn3iv90.0Nb5xvi—Sn4—Nb5xvii150.09 (4)
Sn3ii—Tb1—Sn3iv120.0Nb5v—Sn4—Nb5xvii57.772 (6)
Sn3iii—Tb1—Sn3iv60.0Nb5—Sn4—Tb175.05 (2)
Sn3i—Tb1—Sn3iv120.0Nb5xv—Sn4—Tb175.05 (2)
Sn3—Tb1—Sn3iv60.0Nb5ix—Sn4—Tb175.05 (2)
Sn4—Tb1—Sn3v90.0Nb5xvi—Sn4—Tb175.05 (2)
Sn4i—Tb1—Sn3v90.0Nb5v—Sn4—Tb175.05 (2)
Sn3ii—Tb1—Sn3v60.0Nb5xvii—Sn4—Tb175.05 (2)
Sn3iii—Tb1—Sn3v120.0Nb5—Sn4—Sn4xviii104.95 (2)
Sn3i—Tb1—Sn3v60.0Nb5xv—Sn4—Sn4xviii104.95 (2)
Sn3—Tb1—Sn3v120.0Nb5ix—Sn4—Sn4xviii104.95 (2)
Sn3iv—Tb1—Sn3v180.0Nb5xvi—Sn4—Sn4xviii104.95 (2)
Nb5—Sn2—Nb5vi146.807 (6)Nb5v—Sn4—Sn4xviii104.95 (2)
Nb5—Sn2—Nb5vii110.325 (14)Nb5xvii—Sn4—Sn4xviii104.95 (2)
Nb5vi—Sn2—Nb5vii59.302 (11)Tb1—Sn4—Sn4xviii180.0
Nb5—Sn2—Nb5viii59.302 (11)Nb5viii—Nb5—Nb5xvi180.0
Nb5vi—Sn2—Nb5viii110.325 (14)Nb5viii—Nb5—Nb5ix60.0
Nb5vii—Sn2—Nb5viii146.808 (6)Nb5xvi—Nb5—Nb5ix120.0
Nb5—Sn2—Nb5ix59.302 (11)Nb5viii—Nb5—Nb5xix120.0
Nb5vi—Sn2—Nb5ix146.808 (6)Nb5xvi—Nb5—Nb5xix60.0
Nb5vii—Sn2—Nb5ix146.808 (6)Nb5ix—Nb5—Nb5xix180.0
Nb5viii—Sn2—Nb5ix59.302 (11)Nb5viii—Nb5—Sn360.229 (6)
Nb5—Sn2—Nb5x146.807 (6)Nb5xvi—Nb5—Sn3119.770 (6)
Nb5vi—Sn2—Nb5x59.302 (11)Nb5ix—Nb5—Sn360.229 (6)
Nb5vii—Sn2—Nb5x59.302 (11)Nb5xix—Nb5—Sn3119.770 (6)
Nb5viii—Sn2—Nb5x146.808 (6)Nb5viii—Nb5—Sn3iv119.770 (6)
Nb5ix—Sn2—Nb5x110.325 (14)Nb5xvi—Nb5—Sn3iv60.229 (6)
Nb5viii—Sn3—Nb5iv146.683 (6)Nb5ix—Nb5—Sn3iv119.771 (6)
Nb5viii—Sn3—Nb5xi110.033 (14)Nb5xix—Nb5—Sn3iv60.229 (6)
Nb5iv—Sn3—Nb5xi59.541 (11)Sn3—Nb5—Sn3iv69.967 (14)
Nb5viii—Sn3—Nb5xii146.683 (6)Nb5viii—Nb5—Sn260.349 (6)
Nb5iv—Sn3—Nb5xii59.541 (12)Nb5xvi—Nb5—Sn2119.652 (6)
Nb5xi—Sn3—Nb5xii59.541 (11)Nb5ix—Nb5—Sn260.349 (6)
Nb5viii—Sn3—Nb5ix59.541 (11)Nb5xix—Nb5—Sn2119.652 (6)
Nb5iv—Sn3—Nb5ix146.683 (6)Sn3iv—Nb5—Sn2179.854 (14)
Nb5xi—Sn3—Nb5ix146.683 (6)Nb5viii—Nb5—Sn2vii119.651 (6)
Nb5xii—Sn3—Nb5ix110.033 (14)Nb5xvi—Nb5—Sn2vii60.349 (6)
Nb5viii—Sn3—Nb559.541 (12)Nb5ix—Nb5—Sn2vii119.652 (6)
Nb5iv—Sn3—Nb5110.033 (14)Nb5xix—Nb5—Sn2vii60.349 (6)
Nb5xi—Sn3—Nb5146.683 (6)Sn3—Nb5—Sn2vii179.855 (14)
Nb5xii—Sn3—Nb5146.683 (6)Sn3iv—Nb5—Sn2vii110.179 (2)
Nb5ix—Sn3—Nb559.541 (11)Sn2—Nb5—Sn2vii69.676 (14)
Nb5viii—Sn3—Tb1xiii73.341 (3)Nb5viii—Nb5—Sn4118.886 (3)
Nb5iv—Sn3—Tb1xiii73.341 (3)Nb5xvi—Nb5—Sn461.114 (3)
Nb5xi—Sn3—Tb1xiii73.341 (3)Nb5ix—Nb5—Sn461.114 (3)
Nb5xii—Sn3—Tb1xiii124.984 (7)Nb5xix—Nb5—Sn4118.886 (3)
Nb5ix—Sn3—Tb1xiii124.984 (7)Sn3—Nb5—Sn4102.205 (16)
Nb5—Sn3—Tb1xiii73.341 (3)Sn3iv—Nb5—Sn4102.205 (17)
Nb5viii—Sn3—Tb1xiv73.341 (3)Sn2—Nb5—Sn477.773 (17)
Nb5iv—Sn3—Tb1xiv124.984 (7)Sn2vii—Nb5—Sn477.773 (17)
Nb5xi—Sn3—Tb1xiv73.341 (3)Nb5viii—Nb5—Sn4xiii61.114 (3)
Nb5xii—Sn3—Tb1xiv73.341 (3)Nb5xvi—Nb5—Sn4xiii118.886 (3)
Nb5ix—Sn3—Tb1xiv73.341 (3)Nb5ix—Nb5—Sn4xiii118.886 (3)
Nb5—Sn3—Tb1xiv124.983 (7)Nb5xix—Nb5—Sn4xiii61.114 (3)
Tb1xiii—Sn3—Tb1xiv120.0Sn3—Nb5—Sn4xiii102.205 (17)
Nb5viii—Sn3—Tb1124.984 (7)Sn3iv—Nb5—Sn4xiii102.205 (16)
Nb5iv—Sn3—Tb173.341 (3)Sn2—Nb5—Sn4xiii77.773 (17)
Nb5xi—Sn3—Tb1124.983 (7)Sn2vii—Nb5—Sn4xiii77.772 (17)
Nb5xii—Sn3—Tb173.341 (3)Sn4—Nb5—Sn4xiii150.09 (4)
Nb5ix—Sn3—Tb173.341 (3)
Symmetry codes: (i) x, y, z; (ii) x+1, y+1, z; (iii) x1, y1, z; (iv) x, y+1, z; (v) x, y1, z; (vi) xy+1, x+1, z+1; (vii) x, y+1, z+1; (viii) x+y, x+1, z; (ix) y+1, xy+1, z; (x) y, x+y, z+1; (xi) xy+1, x+1, z; (xii) y, x+y, z; (xiii) x, y+1, z; (xiv) x+1, y+1, z; (xv) y, xy, z; (xvi) x+y1, x, z; (xvii) x+y, x, z; (xviii) x, y, z+1; (xix) y, xy+1, z.

Experimental details

Crystal data
Chemical formulaTbNb6Sn6
Mr1428.52
Crystal system, space groupHexagonal, P6/mmm
Temperature (K)293
a, c (Å)5.7650 (1), 9.5387 (4)
V3)274.55 (1)
Z1
Radiation typeMo Kα
µ (mm1)25.66
Crystal size (mm)0.05 × 0.02 × 0.004
Data collection
DiffractometerOxford Diffraction Xcalibur3
diffractometer with CCD detector
Absorption correctionMulti-scan
(CrysAlis RED, Oxford Diffraction, 2008)
Tmin, Tmax0.592, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
2493, 208, 181
Rint0.027
(sin θ/λ)max1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.017, 0.038, 1.29
No. of reflections208
No. of parameters15
Δρmax, Δρmin (e Å3)1.68, 2.35

Computer programs: CrysAlis CCD (Oxford Diffraction, 2008), CrysAlis RED (Oxford Diffraction, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006), publCIF (Westrip, 2010).

 

Footnotes

Also at Institute of Chemistry, Environment Protection and Biotechnology, Jan Dlugosz University, al. Armii Krajowej 13/15, 42-200 Czestochowa, Poland.

Acknowledgements

IO thanks the DAAD for a grant within the Leonhard-Euler program.

References

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