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

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ISSN: 2056-9890

Crystal structure of Ba5In4Sb6

aState Key Laboratory of Crystal Materials, Institute of Crystal Materials, Shandong University, Jinan, Shandong 250100, People's Republic of China
*Correspondence e-mail: shqxia@sdu.edu.cn

Edited by W. T. A. Harrison, University of Aberdeen, Scotland (Received 11 March 2015; accepted 7 April 2015; online 9 April 2015)

The title compound, penta­barium tetra­indium hexa­anti­mony, was synthesized by an indium-flux reaction and its structure features layers composed of edge-sharing In2Sb6 units. The voids between the In4Sb6 layers are filled by Ba2+ cations, which are all surrounded by six Sb atoms and form bicapped octa­hedral or triangular prismatic coordination geometries. There are five barium ions in the asymmetric unit: one has no imposed crystallographic symmetry, two lie on mirror planes and two have mm2 point symmetry. The two In atoms and four Sb atoms in the asymmetric unit all lie on general crystallographic positions.

1. Related literature

For geometrical details of In—In inter­connections in other structures, see: Iandelli (1964[Iandelli, A. (1964). Z. Anorg. Allg. Chem. 330, 221-232.]); Goforth et al., (2008[Goforth, A. M., Klavins, P., Fettinger, J. C. & Kauzlarich, S. M. (2008). Inorg. Chem. 47, 11048-11056.]).

2. Experimental

2.1. Crystal data

  • Ba5In4Sb6

  • Mr = 1876.48

  • Orthorhombic, P m m n

  • a = 14.2723 (13) Å

  • b = 18.3578 (17) Å

  • c = 8.2710 (8) Å

  • V = 2167.1 (4) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 20.39 mm−1

  • T = 120 K

  • 0.06 × 0.03 × 0.02 mm

2.2. Data collection

  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.374, Tmax = 0.686

  • 12962 measured reflections

  • 2676 independent reflections

  • 2098 reflections with I > 2σ(I)

  • Rint = 0.050

2.3. Refinement

  • R[F2 > 2σ(F2)] = 0.029

  • wR(F2) = 0.055

  • S = 1.02

  • 2676 reflections

  • 79 parameters

  • Δρmax = 2.00 e Å−3

  • Δρmin = −1.69 e Å−3

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

Single crystal of Ba5In4Sb6 was obtained from a high-temperature In-flux reaction and it crystallizes in its own structure type. The layers are constituted by edge-shared In2Sb6 units and stack along the crystallographic b-axis direction. Each In is four-coordinated which is connected by three Sb and the other In atom. All Ba cations are six-coordinated with the bicapped octahedron or triangular prism geometries formed by Sb anions. The bond lengths of In1—In1 and In2—In2 are 2.9655 (11) and 2.8544 (11) Å, respectively, comparable to In—In interconnections in EuIn2As2 (2.765 Å) (Goforth et al., 2008) and CaIn2 (2.92 Å) (Iandelli, 1964).

Related literature top

For geometrical details of In—In interconnections in other structures, see: Iandelli (1964); Goforth et al., (2008).

Experimental top

The title compound was synthesized through the high temperature In flux reaction. All starting elements were handled inside an Argon-filled glove box with controlled oxygen and moisture levels below 0.1 p.p.m.. The reaction conditions were optimized as follows: Ba, In and Sb in a molar ratio of 3:30:5 were loaded in an alumina crucible, which were subsequently flame-sealed in a fused silica tube. The reactants were heated quickly to 1173 K and allowed to dwell at this temperature for 20 h. After a slow cooling process down to 773 K at a rate of 2 K/h, the molten In was removed by centrifugation.

Refinement top

The residual electron densities show a maximum peak of 1.997 e/Å3 and a minimum hole of -1.689 e/Å3, which are 0.78 and 1.58 Å to Ba3 and In1, respectively.

Structure description top

Single crystal of Ba5In4Sb6 was obtained from a high-temperature In-flux reaction and it crystallizes in its own structure type. The layers are constituted by edge-shared In2Sb6 units and stack along the crystallographic b-axis direction. Each In is four-coordinated which is connected by three Sb and the other In atom. All Ba cations are six-coordinated with the bicapped octahedron or triangular prism geometries formed by Sb anions. The bond lengths of In1—In1 and In2—In2 are 2.9655 (11) and 2.8544 (11) Å, respectively, comparable to In—In interconnections in EuIn2As2 (2.765 Å) (Goforth et al., 2008) and CaIn2 (2.92 Å) (Iandelli, 1964).

For geometrical details of In—In interconnections in other structures, see: Iandelli (1964); Goforth et al., (2008).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The ellipsoid of Ba5In4Sb6, viewed along the c-axis. The barium cations, Indium atoms and antimony anions were plotted as yellow, light blue and purple spheres, respectively. Ellipsoids are drawn at the 80% probability level.
Pentabarium tetraindium hexaantimony top
Crystal data top
Ba5In4Sb6F(000) = 3128
Mr = 1876.48Dx = 5.751 Mg m3
Orthorhombic, PmmnMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2aCell parameters from 1832 reflections
a = 14.2723 (13) Åθ = 2.9–27.6°
b = 18.3578 (17) ŵ = 20.39 mm1
c = 8.2710 (8) ÅT = 120 K
V = 2167.1 (4) Å3Block, black
Z = 40.06 × 0.03 × 0.02 mm
Data collection top
Bruker APEXII CCD
diffractometer
2676 independent reflections
Radiation source: fine-focus sealed tube2098 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.050
φ and ω scansθmax = 27.6°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)
h = 1814
Tmin = 0.374, Tmax = 0.686k = 2319
12962 measured reflectionsl = 910
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)] = 0.029 w = 1/[σ2(Fo2) + (0.0146P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055(Δ/σ)max = 0.001
S = 1.02Δρmax = 2.00 e Å3
2676 reflectionsΔρmin = 1.69 e Å3
79 parametersExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.000211 (8)
Crystal data top
Ba5In4Sb6V = 2167.1 (4) Å3
Mr = 1876.48Z = 4
Orthorhombic, PmmnMo Kα radiation
a = 14.2723 (13) ŵ = 20.39 mm1
b = 18.3578 (17) ÅT = 120 K
c = 8.2710 (8) Å0.06 × 0.03 × 0.02 mm
Data collection top
Bruker APEXII CCD
diffractometer
2676 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2005)
2098 reflections with I > 2σ(I)
Tmin = 0.374, Tmax = 0.686Rint = 0.050
12962 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02979 parameters
wR(F2) = 0.0550 restraints
S = 1.02Δρmax = 2.00 e Å3
2676 reflectionsΔρmin = 1.69 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
Ba10.08681 (3)0.00085 (2)0.23996 (5)0.00924 (11)
Ba20.10037 (4)0.25000.26369 (7)0.00879 (14)
Ba30.25000.50189 (3)0.73898 (7)0.00933 (14)
Ba40.25000.75000.07159 (11)0.0113 (2)
Ba50.25000.25000.70687 (10)0.00876 (19)
In10.56473 (4)0.66923 (3)0.10245 (6)0.00979 (13)
In20.59568 (3)0.17226 (3)0.43328 (6)0.00990 (13)
Sb10.07830 (3)0.11748 (3)0.57615 (6)0.00809 (11)
Sb20.58565 (3)0.12044 (3)0.09457 (6)0.00865 (12)
Sb30.25000.12590 (4)0.05576 (8)0.00786 (15)
Sb40.25000.61680 (4)0.39782 (9)0.00841 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ba10.0093 (2)0.0090 (2)0.0094 (2)0.00006 (17)0.00107 (17)0.00072 (18)
Ba20.0094 (3)0.0092 (3)0.0078 (3)0.0000.0016 (2)0.000
Ba30.0094 (3)0.0093 (3)0.0093 (3)0.0000.0000.0005 (2)
Ba40.0116 (5)0.0101 (5)0.0122 (5)0.0000.0000.000
Ba50.0076 (5)0.0095 (4)0.0092 (5)0.0000.0000.000
In10.0105 (3)0.0111 (3)0.0077 (3)0.0025 (2)0.0016 (2)0.0011 (2)
In20.0088 (3)0.0102 (3)0.0107 (3)0.0017 (2)0.0008 (2)0.0008 (2)
Sb10.0087 (3)0.0088 (3)0.0068 (2)0.0004 (2)0.00068 (19)0.00060 (18)
Sb20.0086 (3)0.0092 (3)0.0081 (3)0.0012 (2)0.00116 (19)0.00030 (19)
Sb30.0068 (4)0.0081 (4)0.0087 (4)0.0000.0000.0002 (3)
Sb40.0063 (4)0.0096 (4)0.0093 (4)0.0000.0000.0013 (3)
Geometric parameters (Å, º) top
Ba1—Sb4i3.4343 (7)Ba5—In1xviii3.4173 (7)
Ba1—Sb2ii3.5105 (7)Ba5—In1xix3.4173 (7)
Ba1—Sb13.5115 (7)Ba5—In1xx3.4173 (7)
Ba1—Sb1iii3.5475 (7)Ba5—Sb13.6184 (6)
Ba1—Sb2iv3.5516 (7)Ba5—Sb1i3.6184 (6)
Ba1—Sb33.6077 (7)Ba5—Sb1ix3.6184 (6)
Ba1—In1i3.9649 (7)Ba5—Sb1ii3.6184 (6)
Ba1—Ba24.5821 (6)Ba5—Sb3xii3.6766 (10)
Ba1—Ba1ii4.6582 (10)Ba5—Sb3xxi3.6766 (10)
Ba1—Ba1v4.6795 (9)Ba5—Ba2i4.2423 (10)
Ba1—Ba3i4.7394 (8)In1—Sb1xxii2.8296 (8)
Ba1—Ba3vi4.7537 (8)In1—Sb2xv2.8398 (7)
Ba2—In1vii3.4100 (8)In1—In1xxiii2.9655 (11)
Ba2—In1viii3.4100 (8)In1—Sb3xxiv3.0556 (7)
Ba2—In2ii3.4400 (8)In1—Ba2xxiv3.4100 (8)
Ba2—In2i3.4400 (8)In1—Ba5xvii3.4173 (7)
Ba2—Sb1ix3.5632 (7)In1—Ba1i3.9649 (7)
Ba2—Sb13.5632 (7)In2—Sb4xxv2.7998 (7)
Ba2—Sb3i3.5649 (7)In2—In2ix2.8544 (11)
Ba2—Sb33.5649 (7)In2—Sb1ii2.9279 (7)
Ba2—Sb2ii3.8291 (7)In2—Sb22.9620 (8)
Ba2—Sb2i3.8291 (7)In2—Ba2i3.4400 (8)
Ba2—Ba54.2423 (10)In2—Ba3xxv4.0820 (8)
Ba2—Ba2i4.2711 (13)Sb1—In1xx2.8296 (8)
Ba3—Sb2x3.4833 (7)Sb1—In2ii2.9279 (7)
Ba3—Sb2xi3.4833 (7)Sb1—Ba1iii3.5475 (7)
Ba3—Sb3xii3.5169 (9)Sb1—Ba3i3.5527 (7)
Ba3—Sb43.5230 (9)Sb2—In1xxvi2.8398 (7)
Ba3—Sb1ix3.5527 (7)Sb2—Ba3xxv3.4833 (7)
Ba3—Sb1i3.5527 (7)Sb2—Ba1ii3.5105 (7)
Ba3—In2x4.0820 (8)Sb2—Ba1xxvii3.5516 (7)
Ba3—In2xi4.0820 (8)Sb2—Ba4xiv3.6122 (6)
Ba3—Ba54.6318 (7)Sb2—Ba2i3.8291 (7)
Ba3—Ba1ix4.7394 (8)Sb3—In1vii3.0556 (7)
Ba3—Ba1i4.7394 (8)Sb3—In1xxvi3.0556 (7)
Ba3—Ba1xii4.7537 (8)Sb3—Ba3vi3.5169 (9)
Ba4—Sb2xiii3.6122 (6)Sb3—Ba2i3.5649 (7)
Ba4—Sb2xiv3.6122 (6)Sb3—Ba1ii3.6077 (7)
Ba4—Sb2viii3.6122 (6)Sb3—Ba5xxviii3.6766 (10)
Ba4—Sb2xv3.6122 (6)Sb4—In2x2.7998 (7)
Ba4—Sb4xvi3.6414 (10)Sb4—In2xi2.7998 (7)
Ba4—Sb43.6414 (10)Sb4—Ba1ix3.4343 (7)
Ba5—In1xvii3.4173 (7)Sb4—Ba1i3.4343 (7)
Sb4i—Ba1—Sb2ii177.466 (19)Sb2xiv—Ba4—Sb2viii80.989 (19)
Sb4i—Ba1—Sb196.078 (18)Sb2xiii—Ba4—Sb2xv80.989 (19)
Sb2ii—Ba1—Sb182.282 (15)Sb2xiv—Ba4—Sb2xv82.364 (19)
Sb4i—Ba1—Sb1iii84.397 (16)Sb2viii—Ba4—Sb2xv135.28 (3)
Sb2ii—Ba1—Sb1iii93.674 (16)Sb2xiii—Ba4—Sb4xvi136.392 (16)
Sb1—Ba1—Sb1iii90.625 (16)Sb2xiv—Ba4—Sb4xvi80.779 (13)
Sb4i—Ba1—Sb2iv84.553 (18)Sb2viii—Ba4—Sb4xvi80.780 (13)
Sb2ii—Ba1—Sb2iv97.002 (15)Sb2xv—Ba4—Sb4xvi136.392 (16)
Sb1—Ba1—Sb2iv177.436 (18)Sb2xiii—Ba4—Sb480.780 (13)
Sb1iii—Ba1—Sb2iv86.962 (15)Sb2xiv—Ba4—Sb4136.392 (16)
Sb4i—Ba1—Sb397.059 (16)Sb2viii—Ba4—Sb4136.392 (16)
Sb2ii—Ba1—Sb384.841 (15)Sb2xv—Ba4—Sb480.779 (13)
Sb1—Ba1—Sb388.211 (17)Sb4xvi—Ba4—Sb484.37 (3)
Sb1iii—Ba1—Sb3178.223 (18)In1xvii—Ba5—In1xviii101.39 (2)
Sb2iv—Ba1—Sb394.182 (17)In1xvii—Ba5—In1xix51.430 (19)
Sb4i—Ba1—In1i89.069 (17)In1xviii—Ba5—In1xix125.03 (3)
Sb2ii—Ba1—In1i90.672 (16)In1xvii—Ba5—In1xx125.03 (3)
Sb1—Ba1—In1i133.506 (16)In1xviii—Ba5—In1xx51.430 (19)
Sb1iii—Ba1—In1i43.815 (13)In1xix—Ba5—In1xx101.39 (2)
Sb2iv—Ba1—In1i43.967 (12)In1xvii—Ba5—Sb1162.493 (19)
Sb3—Ba1—In1i137.062 (18)In1xviii—Ba5—Sb184.581 (13)
Sb4i—Ba1—Ba2125.651 (17)In1xix—Ba5—Sb1111.730 (13)
Sb2ii—Ba1—Ba254.554 (13)In1xx—Ba5—Sb147.322 (13)
Sb1—Ba1—Ba250.129 (13)In1xvii—Ba5—Sb1i47.322 (13)
Sb1iii—Ba1—Ba2128.386 (16)In1xviii—Ba5—Sb1i111.730 (13)
Sb2iv—Ba1—Ba2131.250 (16)In1xix—Ba5—Sb1i84.581 (13)
Sb3—Ba1—Ba249.885 (14)In1xx—Ba5—Sb1i162.493 (19)
In1i—Ba1—Ba2145.225 (16)Sb1—Ba5—Sb1i145.23 (3)
Sb4i—Ba1—Ba1ii47.298 (11)In1xvii—Ba5—Sb1ix111.730 (13)
Sb2ii—Ba1—Ba1ii134.518 (11)In1xviii—Ba5—Sb1ix47.322 (13)
Sb1—Ba1—Ba1ii91.983 (11)In1xix—Ba5—Sb1ix162.493 (19)
Sb1iii—Ba1—Ba1ii131.624 (11)In1xx—Ba5—Sb1ix84.581 (13)
Sb2iv—Ba1—Ba1ii90.267 (10)Sb1—Ba5—Sb1ix84.494 (18)
Sb3—Ba1—Ba1ii49.790 (10)Sb1i—Ba5—Sb1ix85.261 (18)
In1i—Ba1—Ba1ii123.058 (10)In1xvii—Ba5—Sb1ii84.581 (13)
Ba2—Ba1—Ba1ii87.579 (9)In1xviii—Ba5—Sb1ii162.493 (19)
Sb4i—Ba1—Ba1v132.64 (2)In1xix—Ba5—Sb1ii47.322 (13)
Sb2ii—Ba1—Ba1v48.878 (11)In1xx—Ba5—Sb1ii111.730 (13)
Sb1—Ba1—Ba1v131.107 (18)Sb1—Ba5—Sb1ii85.261 (18)
Sb1iii—Ba1—Ba1v90.449 (16)Sb1i—Ba5—Sb1ii84.494 (18)
Sb2iv—Ba1—Ba1v48.124 (12)Sb1ix—Ba5—Sb1ii145.23 (3)
Sb3—Ba1—Ba1v89.306 (16)In1xvii—Ba5—Sb3xii50.868 (13)
In1i—Ba1—Ba1v57.489 (12)In1xviii—Ba5—Sb3xii50.868 (13)
Ba2—Ba1—Ba1v93.748 (14)In1xix—Ba5—Sb3xii84.64 (2)
Ba1ii—Ba1—Ba1v121.973 (11)In1xx—Ba5—Sb3xii84.64 (2)
Sb4i—Ba1—Ba3i47.852 (14)Sb1—Ba5—Sb3xii130.627 (17)
Sb2ii—Ba1—Ba3i130.506 (15)Sb1i—Ba5—Sb3xii79.508 (13)
Sb1—Ba1—Ba3i48.233 (12)Sb1ix—Ba5—Sb3xii79.508 (13)
Sb1iii—Ba1—Ba3i86.937 (14)Sb1ii—Ba5—Sb3xii130.627 (17)
Sb2iv—Ba1—Ba3i132.382 (15)In1xvii—Ba5—Sb3xxi84.64 (2)
Sb3—Ba1—Ba3i93.283 (15)In1xviii—Ba5—Sb3xxi84.64 (2)
In1i—Ba1—Ba3i120.632 (14)In1xix—Ba5—Sb3xxi50.868 (13)
Ba2—Ba1—Ba3i87.281 (13)In1xx—Ba5—Sb3xxi50.868 (13)
Ba1ii—Ba1—Ba3i60.565 (7)Sb1—Ba5—Sb3xxi79.508 (13)
Ba1v—Ba1—Ba3i177.275 (17)Sb1i—Ba5—Sb3xxi130.627 (17)
Sb4i—Ba1—Ba3vi89.567 (16)Sb1ix—Ba5—Sb3xxi130.627 (17)
Sb2ii—Ba1—Ba3vi92.956 (14)Sb1ii—Ba5—Sb3xxi79.508 (13)
Sb1—Ba1—Ba3vi135.534 (16)Sb3xii—Ba5—Sb3xxi76.58 (3)
Sb1iii—Ba1—Ba3vi133.841 (15)In1xvii—Ba5—Ba2142.027 (19)
Sb2iv—Ba1—Ba3vi46.886 (12)In1xviii—Ba5—Ba290.531 (15)
Sb3—Ba1—Ba3vi47.337 (14)In1xix—Ba5—Ba2142.027 (19)
In1i—Ba1—Ba3vi90.508 (13)In1xx—Ba5—Ba290.531 (15)
Ba2—Ba1—Ba3vi91.559 (13)Sb1—Ba5—Ba253.194 (13)
Ba1ii—Ba1—Ba3vi60.662 (7)Sb1i—Ba5—Ba294.75 (2)
Ba1v—Ba1—Ba3vi61.312 (12)Sb1ix—Ba5—Ba253.194 (13)
Ba3i—Ba1—Ba3vi121.212 (11)Sb1ii—Ba5—Ba294.75 (2)
In1vii—Ba2—In1viii51.55 (2)Sb3xii—Ba5—Ba2132.701 (10)
In1vii—Ba2—In2ii93.462 (18)Sb3xxi—Ba5—Ba2132.701 (10)
In1viii—Ba2—In2ii114.91 (2)In1xvii—Ba5—Ba2i90.531 (15)
In1vii—Ba2—In2i114.91 (2)In1xviii—Ba5—Ba2i142.027 (19)
In1viii—Ba2—In2i93.462 (18)In1xix—Ba5—Ba2i90.531 (15)
In2ii—Ba2—In2i49.02 (2)In1xx—Ba5—Ba2i142.027 (19)
In1vii—Ba2—Sb1ix158.09 (2)Sb1—Ba5—Ba2i94.75 (2)
In1viii—Ba2—Sb1ix109.515 (14)Sb1i—Ba5—Ba2i53.194 (13)
In2ii—Ba2—Sb1ix85.158 (18)Sb1ix—Ba5—Ba2i94.75 (2)
In2i—Ba2—Sb1ix49.389 (14)Sb1ii—Ba5—Ba2i53.194 (13)
In1vii—Ba2—Sb1109.515 (14)Sb3xii—Ba5—Ba2i132.701 (10)
In1viii—Ba2—Sb1158.09 (2)Sb3xxi—Ba5—Ba2i132.701 (10)
In2ii—Ba2—Sb149.389 (14)Ba2—Ba5—Ba2i60.45 (2)
In2i—Ba2—Sb185.158 (18)Sb1xxii—In1—Sb2xv119.01 (2)
Sb1ix—Ba2—Sb186.12 (2)Sb1xxii—In1—In1xxiii109.617 (14)
In1vii—Ba2—Sb3i86.49 (2)Sb2xv—In1—In1xxiii108.387 (14)
In1viii—Ba2—Sb3i51.906 (14)Sb1xxii—In1—Sb3xxiv104.82 (2)
In2ii—Ba2—Sb3i161.643 (18)Sb2xv—In1—Sb3xxiv109.04 (2)
In2i—Ba2—Sb3i114.761 (14)In1xxiii—In1—Sb3xxiv105.090 (16)
Sb1ix—Ba2—Sb3i88.083 (16)Sb1xxii—In1—Ba2xxiv165.95 (2)
Sb1—Ba2—Sb3i147.05 (2)Sb2xv—In1—Ba2xxiv74.947 (19)
In1vii—Ba2—Sb351.906 (14)In1xxiii—In1—Ba2xxiv64.226 (10)
In1viii—Ba2—Sb386.49 (2)Sb3xxiv—In1—Ba2xxiv66.660 (19)
In2ii—Ba2—Sb3114.761 (14)Sb1xxii—In1—Ba5xvii70.071 (19)
In2i—Ba2—Sb3161.643 (18)Sb2xv—In1—Ba5xvii170.58 (2)
Sb1ix—Ba2—Sb3147.05 (2)In1xxiii—In1—Ba5xvii64.285 (10)
Sb1—Ba2—Sb388.083 (16)Sb3xxiv—In1—Ba5xvii68.962 (19)
Sb3i—Ba2—Sb379.45 (2)Ba2xxiv—In1—Ba5xvii96.07 (2)
In1vii—Ba2—Sb2ii45.739 (13)Sb1xxii—In1—Ba1i60.226 (15)
In1viii—Ba2—Sb2ii80.925 (18)Sb2xv—In1—Ba1i60.260 (15)
In2ii—Ba2—Sb2ii47.723 (14)In1xxiii—In1—Ba1i141.952 (10)
In2i—Ba2—Sb2ii80.950 (18)Sb3xxiv—In1—Ba1i112.95 (2)
Sb1ix—Ba2—Sb2ii128.88 (2)Ba2xxiv—In1—Ba1i132.730 (18)
Sb1—Ba2—Sb2ii77.265 (13)Ba5xvii—In1—Ba1i129.15 (2)
Sb3i—Ba2—Sb2ii129.50 (2)Sb4xxv—In2—In2ix111.322 (17)
Sb3—Ba2—Sb2ii80.918 (14)Sb4xxv—In2—Sb1ii109.93 (2)
In1vii—Ba2—Sb2i80.925 (18)In2ix—In2—Sb1ii110.086 (14)
In1viii—Ba2—Sb2i45.739 (13)Sb4xxv—In2—Sb2113.15 (2)
In2ii—Ba2—Sb2i80.950 (18)In2ix—In2—Sb2108.733 (14)
In2i—Ba2—Sb2i47.723 (14)Sb1ii—In2—Sb2103.32 (2)
Sb1ix—Ba2—Sb2i77.265 (13)Sb4xxv—In2—Ba2i173.81 (3)
Sb1—Ba2—Sb2i128.88 (2)In2ix—In2—Ba2i65.488 (10)
Sb3i—Ba2—Sb2i80.918 (14)Sb1ii—In2—Ba2i67.497 (17)
Sb3—Ba2—Sb2i129.50 (2)Sb2—In2—Ba2i73.039 (18)
Sb2ii—Ba2—Sb2i76.80 (2)Sb4xxv—In2—Ba3xxv58.068 (19)
In1vii—Ba2—Ba5147.398 (15)In2ix—In2—Ba3xxv140.012 (10)
In1viii—Ba2—Ba5147.398 (15)Sb1ii—In2—Ba3xxv109.592 (19)
In2ii—Ba2—Ba593.275 (18)Sb2—In2—Ba3xxv56.626 (15)
In2i—Ba2—Ba593.275 (18)Ba2i—In2—Ba3xxv127.911 (18)
Sb1ix—Ba2—Ba554.396 (13)In1xx—Sb1—In2ii101.88 (2)
Sb1—Ba2—Ba554.396 (13)In1xx—Sb1—Ba1161.99 (2)
Sb3i—Ba2—Ba596.619 (17)In2ii—Sb1—Ba185.363 (18)
Sb3—Ba2—Ba596.619 (17)In1xx—Sb1—Ba1iii75.959 (17)
Sb2ii—Ba2—Ba5131.656 (13)In2ii—Sb1—Ba1iii79.632 (17)
Sb2i—Ba2—Ba5131.656 (13)Ba1—Sb1—Ba1iii89.375 (16)
In1vii—Ba2—Ba2i98.579 (14)In1xx—Sb1—Ba3i84.155 (19)
In1viii—Ba2—Ba2i98.579 (14)In2ii—Sb1—Ba3i161.77 (2)
In2ii—Ba2—Ba2i144.428 (13)Ba1—Sb1—Ba3i84.272 (16)
In2i—Ba2—Ba2i144.428 (13)Ba1iii—Sb1—Ba3i85.293 (16)
Sb1ix—Ba2—Ba2i95.073 (13)In1xx—Sb1—Ba2117.27 (2)
Sb1—Ba2—Ba2i95.073 (13)In2ii—Sb1—Ba263.114 (17)
Sb3i—Ba2—Ba2i53.198 (11)Ba1—Sb1—Ba280.729 (16)
Sb3—Ba2—Ba2i53.198 (11)Ba1iii—Sb1—Ba2141.977 (19)
Sb2ii—Ba2—Ba2i133.895 (11)Ba3i—Sb1—Ba2129.426 (19)
Sb2i—Ba2—Ba2i133.895 (11)In1xx—Sb1—Ba562.606 (19)
Ba5—Ba2—Ba2i59.775 (11)In2ii—Sb1—Ba5117.648 (19)
Sb2x—Ba3—Sb2xi84.66 (2)Ba1—Sb1—Ba5128.543 (19)
Sb2x—Ba3—Sb3xii97.024 (18)Ba1iii—Sb1—Ba5137.18 (2)
Sb2xi—Ba3—Sb3xii97.024 (18)Ba3i—Sb1—Ba580.461 (15)
Sb2x—Ba3—Sb486.702 (17)Ba2—Sb1—Ba572.411 (18)
Sb2xi—Ba3—Sb486.702 (17)In1xxvi—Sb2—In2118.55 (2)
Sb3xii—Ba3—Sb4174.94 (2)In1xxvi—Sb2—Ba3xxv158.88 (2)
Sb2x—Ba3—Sb1ix178.605 (18)In2—Sb2—Ba3xxv78.130 (18)
Sb2xi—Ba3—Sb1ix94.053 (13)In1xxvi—Sb2—Ba1ii82.178 (18)
Sb3xii—Ba3—Sb1ix82.585 (17)In2—Sb2—Ba1ii84.879 (18)
Sb4—Ba3—Sb1ix93.769 (17)Ba3xxv—Sb2—Ba1ii86.909 (16)
Sb2x—Ba3—Sb1i94.053 (13)In1xxvi—Sb2—Ba1xxvii75.772 (18)
Sb2xi—Ba3—Sb1i178.605 (18)In2—Sb2—Ba1xxvii159.71 (2)
Sb3xii—Ba3—Sb1i82.585 (17)Ba3xxv—Sb2—Ba1xxvii85.014 (17)
Sb4—Ba3—Sb1i93.769 (17)Ba1ii—Sb2—Ba1xxvii82.998 (15)
Sb1ix—Ba3—Sb1i87.23 (2)In1xxvi—Sb2—Ba4xiv93.71 (2)
Sb2x—Ba3—In2x45.244 (13)In2—Sb2—Ba4xiv96.72 (2)
Sb2xi—Ba3—In2x91.297 (18)Ba3xxv—Sb2—Ba4xiv97.149 (16)
Sb3xii—Ba3—In2x140.454 (14)Ba1ii—Sb2—Ba4xiv175.863 (18)
Sb4—Ba3—In2x42.412 (12)Ba1xxvii—Sb2—Ba4xiv96.509 (19)
Sb1ix—Ba3—In2x135.44 (2)In1xxvi—Sb2—Ba2i59.314 (17)
Sb1i—Ba3—In2x88.172 (14)In2—Sb2—Ba2i59.238 (16)
Sb2x—Ba3—In2xi91.297 (18)Ba3xxv—Sb2—Ba2i135.28 (2)
Sb2xi—Ba3—In2xi45.244 (13)Ba1ii—Sb2—Ba2i77.125 (15)
Sb3xii—Ba3—In2xi140.454 (14)Ba1xxvii—Sb2—Ba2i132.629 (18)
Sb4—Ba3—In2xi42.412 (12)Ba4xiv—Sb2—Ba2i100.382 (15)
Sb1ix—Ba3—In2xi88.172 (14)In1vii—Sb3—In1xxvi119.85 (3)
Sb1i—Ba3—In2xi135.44 (2)In1vii—Sb3—Ba3vi81.640 (18)
In2x—Ba3—In2xi65.310 (18)In1xxvi—Sb3—Ba3vi81.641 (18)
Sb2x—Ba3—Ba5130.270 (14)In1vii—Sb3—Ba2i123.96 (2)
Sb2xi—Ba3—Ba5130.270 (14)In1xxvi—Sb3—Ba2i61.434 (16)
Sb3xii—Ba3—Ba551.447 (18)Ba3vi—Sb3—Ba2i141.785 (14)
Sb4—Ba3—Ba5123.49 (2)In1vii—Sb3—Ba261.434 (16)
Sb1ix—Ba3—Ba550.390 (12)In1xxvi—Sb3—Ba2123.96 (2)
Sb1i—Ba3—Ba550.390 (12)Ba3vi—Sb3—Ba2141.785 (14)
In2x—Ba3—Ba5138.151 (14)Ba2i—Sb3—Ba273.60 (2)
In2xi—Ba3—Ba5138.151 (14)In1vii—Sb3—Ba177.750 (14)
Sb2x—Ba3—Ba1ix132.982 (18)In1xxvi—Sb3—Ba1154.85 (2)
Sb2xi—Ba3—Ba1ix91.140 (13)Ba3vi—Sb3—Ba183.695 (17)
Sb3xii—Ba3—Ba1ix129.919 (16)Ba2i—Sb3—Ba1126.13 (2)
Sb4—Ba3—Ba1ix46.281 (12)Ba2—Sb3—Ba179.407 (14)
Sb1ix—Ba3—Ba1ix47.495 (11)In1vii—Sb3—Ba1ii154.85 (2)
Sb1i—Ba3—Ba1ix90.133 (16)In1xxvi—Sb3—Ba1ii77.750 (14)
In2x—Ba3—Ba1ix88.244 (15)Ba3vi—Sb3—Ba1ii83.695 (17)
In2xi—Ba3—Ba1ix55.877 (11)Ba2i—Sb3—Ba1ii79.407 (14)
Ba5—Ba3—Ba1ix86.529 (14)Ba2—Sb3—Ba1ii126.13 (2)
Sb2x—Ba3—Ba1i91.140 (13)Ba1—Sb3—Ba1ii80.42 (2)
Sb2xi—Ba3—Ba1i132.982 (18)In1vii—Sb3—Ba5xxviii60.170 (15)
Sb3xii—Ba3—Ba1i129.919 (16)In1xxvi—Sb3—Ba5xxviii60.170 (15)
Sb4—Ba3—Ba1i46.281 (12)Ba3vi—Sb3—Ba5xxviii80.13 (2)
Sb1ix—Ba3—Ba1i90.133 (16)Ba2i—Sb3—Ba5xxviii89.005 (18)
Sb1i—Ba3—Ba1i47.495 (11)Ba2—Sb3—Ba5xxviii89.005 (18)
In2x—Ba3—Ba1i55.877 (11)Ba1—Sb3—Ba5xxviii136.530 (13)
In2xi—Ba3—Ba1i88.244 (15)Ba1ii—Sb3—Ba5xxviii136.530 (13)
Ba5—Ba3—Ba1i86.529 (14)In2x—Sb4—In2xi103.75 (3)
Ba1ix—Ba3—Ba1i58.870 (14)In2x—Sb4—Ba1ix162.15 (3)
Sb2x—Ba3—Ba1xii48.100 (12)In2xi—Sb4—Ba1ix83.388 (15)
Sb2xi—Ba3—Ba1xii89.545 (17)In2x—Sb4—Ba1i83.388 (15)
Sb3xii—Ba3—Ba1xii48.968 (13)In2xi—Sb4—Ba1i162.15 (3)
Sb4—Ba3—Ba1xii134.789 (16)Ba1ix—Sb4—Ba1i85.40 (2)
Sb1ix—Ba3—Ba1xii131.442 (18)In2x—Sb4—Ba379.52 (2)
Sb1i—Ba3—Ba1xii89.193 (13)In2xi—Sb4—Ba379.52 (2)
In2x—Ba3—Ba1xii92.751 (13)Ba1ix—Sb4—Ba385.867 (17)
In2xi—Ba3—Ba1xii125.221 (17)Ba1i—Sb4—Ba385.867 (17)
Ba5—Ba3—Ba1xii92.258 (15)In2x—Sb4—Ba497.21 (2)
Ba1ix—Ba3—Ba1xii178.779 (18)In2xi—Sb4—Ba497.21 (2)
Ba1i—Ba3—Ba1xii121.212 (11)Ba1ix—Sb4—Ba498.083 (19)
Sb2xiii—Ba4—Sb2xiv135.28 (3)Ba1i—Sb4—Ba498.083 (19)
Sb2xiii—Ba4—Sb2viii82.364 (19)Ba3—Sb4—Ba4174.60 (3)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x+1/2, y, z; (iii) x, y, z+1; (iv) x1/2, y, z; (v) x, y, z; (vi) x+1/2, y+1/2, z1; (vii) x1/2, y1/2, z; (viii) x1/2, y+1, z; (ix) x, y+1/2, z; (x) x+1, y+1/2, z+1; (xi) x1/2, y+1/2, z+1; (xii) x+1/2, y+1/2, z+1; (xiii) x1/2, y+1/2, z; (xiv) x+1, y+1, z; (xv) x+1, y+1/2, z; (xvi) x+1/2, y+3/2, z; (xvii) x+1, y+1, z+1; (xviii) x1/2, y+1, z+1; (xix) x+1, y1/2, z+1; (xx) x1/2, y1/2, z+1; (xxi) x, y, z+1; (xxii) x+1/2, y+1/2, z+1; (xxiii) x, y+3/2, z; (xxiv) x+1/2, y+1/2, z; (xxv) x+1/2, y1/2, z+1; (xxvi) x+1, y1/2, z; (xxvii) x+1/2, y, z; (xxviii) x, y, z1.

Experimental details

Crystal data
Chemical formulaBa5In4Sb6
Mr1876.48
Crystal system, space groupOrthorhombic, Pmmn
Temperature (K)120
a, b, c (Å)14.2723 (13), 18.3578 (17), 8.2710 (8)
V3)2167.1 (4)
Z4
Radiation typeMo Kα
µ (mm1)20.39
Crystal size (mm)0.06 × 0.03 × 0.02
Data collection
DiffractometerBruker APEXII CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2005)
Tmin, Tmax0.374, 0.686
No. of measured, independent and
observed [I > 2σ(I)] reflections
12962, 2676, 2098
Rint0.050
(sin θ/λ)max1)0.651
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.055, 1.02
No. of reflections2676
No. of parameters79
Δρmax, Δρmin (e Å3)2.00, 1.69

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

The authors acknowledges financial support of the National Natural Science Foundation of China (grany No. 51271098).

References

First citationBruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationGoforth, A. M., Klavins, P., Fettinger, J. C. & Kauzlarich, S. M. (2008). Inorg. Chem. 47, 11048–11056.  Web of Science CrossRef PubMed CAS Google Scholar
First citationIandelli, A. (1964). Z. Anorg. Allg. Chem. 330, 221–232.  CrossRef CAS Web of Science Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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