Crystal structure of Ba5In4Sb6

Pan, M.-Y.; Xia, S.-Q.; Tao, X.-T.

doi:10.1107/S2056989015006933

inorganic compounds

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Volume 71| Part 5| May 2015| Page i4

https://doi.org/10.1107/S2056989015006933

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Crystal structure of Ba₅In₄Sb₆

Ming-Yan Pan,^a Sheng-Qing Xia ^a ^* and Xu-Tang Tao ^a

^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.

Keywords: crystal structure; barium; indium; antimony; In—In interconnections.

CCDC reference: 1058152

1. Related literature

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

2. Experimental

2.1. Crystal data

Ba₅In₄Sb₆
M_r = 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 ) T_min = 0.374, T_max = 0.686
12962 measured reflections
2676 independent reflections
2098 reflections with I > 2σ(I)
R_int = 0.050

2.3. Refinement

R[F² > 2σ(F²)] = 0.029
wR(F²) = 0.055
S = 1.02
2676 reflections
79 parameters
Δρ_max = 2.00 e Å⁻³
Δρ_min = −1.69 e Å⁻³

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; 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.

Supporting information

CCDC reference: 1058152

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S2056989015006933/hb7382sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989015006933/hb7382Isup2.hkl

checkCIF report

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.

Structure description top

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

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

Ba₅In₄Sb₆	F(000) = 3128
M_r = 1876.48	D_x = 5.751 Mg m⁻³
Orthorhombic, Pmmn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2a	Cell parameters from 1832 reflections
a = 14.2723 (13) Å	θ = 2.9–27.6°
b = 18.3578 (17) Å	µ = 20.39 mm⁻¹
c = 8.2710 (8) Å	T = 120 K
V = 2167.1 (4) Å³	Block, black
Z = 4	0.06 × 0.03 × 0.02 mm

Data collection top

Bruker APEXII CCD diffractometer	2676 independent reflections
Radiation source: fine-focus sealed tube	2098 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.050
φ and ω scans	θ_max = 27.6°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −18→14
T_min = 0.374, T_max = 0.686	k = −23→19
12962 measured reflections	l = −9→10

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)] = 0.029	w = 1/[σ²(F_o²) + (0.0146P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.055	(Δ/σ)_max = 0.001
S = 1.02	Δρ_max = 2.00 e Å⁻³
2676 reflections	Δρ_min = −1.69 e Å⁻³
79 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.000211 (8)

Crystal data top

Ba₅In₄Sb₆	V = 2167.1 (4) Å³
M_r = 1876.48	Z = 4
Orthorhombic, Pmmn	Mo Kα radiation
a = 14.2723 (13) Å	µ = 20.39 mm⁻¹
b = 18.3578 (17) Å	T = 120 K
c = 8.2710 (8) Å	0.06 × 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)
T_min = 0.374, T_max = 0.686	R_int = 0.050
12962 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	79 parameters
wR(F²) = 0.055	0 restraints
S = 1.02	Δρ_max = 2.00 e Å⁻³
2676 reflections	Δρ_min = −1.69 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
Ba1	0.08681 (3)	0.00085 (2)	0.23996 (5)	0.00924 (11)
Ba2	0.10037 (4)	0.2500	0.26369 (7)	0.00879 (14)
Ba3	0.2500	0.50189 (3)	0.73898 (7)	0.00933 (14)
Ba4	0.2500	0.7500	0.07159 (11)	0.0113 (2)
Ba5	0.2500	0.2500	0.70687 (10)	0.00876 (19)
In1	0.56473 (4)	0.66923 (3)	0.10245 (6)	0.00979 (13)
In2	0.59568 (3)	0.17226 (3)	0.43328 (6)	0.00990 (13)
Sb1	0.07830 (3)	0.11748 (3)	0.57615 (6)	0.00809 (11)
Sb2	0.58565 (3)	0.12044 (3)	0.09457 (6)	0.00865 (12)
Sb3	0.2500	0.12590 (4)	0.05576 (8)	0.00786 (15)
Sb4	0.2500	0.61680 (4)	0.39782 (9)	0.00841 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ba1	0.0093 (2)	0.0090 (2)	0.0094 (2)	0.00006 (17)	−0.00107 (17)	0.00072 (18)
Ba2	0.0094 (3)	0.0092 (3)	0.0078 (3)	0.000	0.0016 (2)	0.000
Ba3	0.0094 (3)	0.0093 (3)	0.0093 (3)	0.000	0.000	0.0005 (2)
Ba4	0.0116 (5)	0.0101 (5)	0.0122 (5)	0.000	0.000	0.000
Ba5	0.0076 (5)	0.0095 (4)	0.0092 (5)	0.000	0.000	0.000
In1	0.0105 (3)	0.0111 (3)	0.0077 (3)	−0.0025 (2)	−0.0016 (2)	0.0011 (2)
In2	0.0088 (3)	0.0102 (3)	0.0107 (3)	0.0017 (2)	−0.0008 (2)	0.0008 (2)
Sb1	0.0087 (3)	0.0088 (3)	0.0068 (2)	0.0004 (2)	−0.00068 (19)	−0.00060 (18)
Sb2	0.0086 (3)	0.0092 (3)	0.0081 (3)	0.0012 (2)	−0.00116 (19)	−0.00030 (19)
Sb3	0.0068 (4)	0.0081 (4)	0.0087 (4)	0.000	0.000	−0.0002 (3)
Sb4	0.0063 (4)	0.0096 (4)	0.0093 (4)	0.000	0.000	−0.0013 (3)

Geometric parameters (Å, º) top

Ba1—Sb4ⁱ	3.4343 (7)	Ba5—In1^xviii	3.4173 (7)
Ba1—Sb2ⁱⁱ	3.5105 (7)	Ba5—In1^xix	3.4173 (7)
Ba1—Sb1	3.5115 (7)	Ba5—In1^xx	3.4173 (7)
Ba1—Sb1ⁱⁱⁱ	3.5475 (7)	Ba5—Sb1	3.6184 (6)
Ba1—Sb2^iv	3.5516 (7)	Ba5—Sb1ⁱ	3.6184 (6)
Ba1—Sb3	3.6077 (7)	Ba5—Sb1^ix	3.6184 (6)
Ba1—In1ⁱ	3.9649 (7)	Ba5—Sb1ⁱⁱ	3.6184 (6)
Ba1—Ba2	4.5821 (6)	Ba5—Sb3^xii	3.6766 (10)
Ba1—Ba1ⁱⁱ	4.6582 (10)	Ba5—Sb3^xxi	3.6766 (10)
Ba1—Ba1^v	4.6795 (9)	Ba5—Ba2ⁱ	4.2423 (10)
Ba1—Ba3ⁱ	4.7394 (8)	In1—Sb1^xxii	2.8296 (8)
Ba1—Ba3^vi	4.7537 (8)	In1—Sb2^xv	2.8398 (7)
Ba2—In1^vii	3.4100 (8)	In1—In1^xxiii	2.9655 (11)
Ba2—In1^viii	3.4100 (8)	In1—Sb3^xxiv	3.0556 (7)
Ba2—In2ⁱⁱ	3.4400 (8)	In1—Ba2^xxiv	3.4100 (8)
Ba2—In2ⁱ	3.4400 (8)	In1—Ba5^xvii	3.4173 (7)
Ba2—Sb1^ix	3.5632 (7)	In1—Ba1ⁱ	3.9649 (7)
Ba2—Sb1	3.5632 (7)	In2—Sb4^xxv	2.7998 (7)
Ba2—Sb3ⁱ	3.5649 (7)	In2—In2^ix	2.8544 (11)
Ba2—Sb3	3.5649 (7)	In2—Sb1ⁱⁱ	2.9279 (7)
Ba2—Sb2ⁱⁱ	3.8291 (7)	In2—Sb2	2.9620 (8)
Ba2—Sb2ⁱ	3.8291 (7)	In2—Ba2ⁱ	3.4400 (8)
Ba2—Ba5	4.2423 (10)	In2—Ba3^xxv	4.0820 (8)
Ba2—Ba2ⁱ	4.2711 (13)	Sb1—In1^xx	2.8296 (8)
Ba3—Sb2^x	3.4833 (7)	Sb1—In2ⁱⁱ	2.9279 (7)
Ba3—Sb2^xi	3.4833 (7)	Sb1—Ba1ⁱⁱⁱ	3.5475 (7)
Ba3—Sb3^xii	3.5169 (9)	Sb1—Ba3ⁱ	3.5527 (7)
Ba3—Sb4	3.5230 (9)	Sb2—In1^xxvi	2.8398 (7)
Ba3—Sb1^ix	3.5527 (7)	Sb2—Ba3^xxv	3.4833 (7)
Ba3—Sb1ⁱ	3.5527 (7)	Sb2—Ba1ⁱⁱ	3.5105 (7)
Ba3—In2^x	4.0820 (8)	Sb2—Ba1^xxvii	3.5516 (7)
Ba3—In2^xi	4.0820 (8)	Sb2—Ba4^xiv	3.6122 (6)
Ba3—Ba5	4.6318 (7)	Sb2—Ba2ⁱ	3.8291 (7)
Ba3—Ba1^ix	4.7394 (8)	Sb3—In1^vii	3.0556 (7)
Ba3—Ba1ⁱ	4.7394 (8)	Sb3—In1^xxvi	3.0556 (7)
Ba3—Ba1^xii	4.7537 (8)	Sb3—Ba3^vi	3.5169 (9)
Ba4—Sb2^xiii	3.6122 (6)	Sb3—Ba2ⁱ	3.5649 (7)
Ba4—Sb2^xiv	3.6122 (6)	Sb3—Ba1ⁱⁱ	3.6077 (7)
Ba4—Sb2^viii	3.6122 (6)	Sb3—Ba5^xxviii	3.6766 (10)
Ba4—Sb2^xv	3.6122 (6)	Sb4—In2^x	2.7998 (7)
Ba4—Sb4^xvi	3.6414 (10)	Sb4—In2^xi	2.7998 (7)
Ba4—Sb4	3.6414 (10)	Sb4—Ba1^ix	3.4343 (7)
Ba5—In1^xvii	3.4173 (7)	Sb4—Ba1ⁱ	3.4343 (7)

Sb4ⁱ—Ba1—Sb2ⁱⁱ	177.466 (19)	Sb2^xiv—Ba4—Sb2^viii	80.989 (19)
Sb4ⁱ—Ba1—Sb1	96.078 (18)	Sb2^xiii—Ba4—Sb2^xv	80.989 (19)
Sb2ⁱⁱ—Ba1—Sb1	82.282 (15)	Sb2^xiv—Ba4—Sb2^xv	82.364 (19)
Sb4ⁱ—Ba1—Sb1ⁱⁱⁱ	84.397 (16)	Sb2^viii—Ba4—Sb2^xv	135.28 (3)
Sb2ⁱⁱ—Ba1—Sb1ⁱⁱⁱ	93.674 (16)	Sb2^xiii—Ba4—Sb4^xvi	136.392 (16)
Sb1—Ba1—Sb1ⁱⁱⁱ	90.625 (16)	Sb2^xiv—Ba4—Sb4^xvi	80.779 (13)
Sb4ⁱ—Ba1—Sb2^iv	84.553 (18)	Sb2^viii—Ba4—Sb4^xvi	80.780 (13)
Sb2ⁱⁱ—Ba1—Sb2^iv	97.002 (15)	Sb2^xv—Ba4—Sb4^xvi	136.392 (16)
Sb1—Ba1—Sb2^iv	177.436 (18)	Sb2^xiii—Ba4—Sb4	80.780 (13)
Sb1ⁱⁱⁱ—Ba1—Sb2^iv	86.962 (15)	Sb2^xiv—Ba4—Sb4	136.392 (16)
Sb4ⁱ—Ba1—Sb3	97.059 (16)	Sb2^viii—Ba4—Sb4	136.392 (16)
Sb2ⁱⁱ—Ba1—Sb3	84.841 (15)	Sb2^xv—Ba4—Sb4	80.779 (13)
Sb1—Ba1—Sb3	88.211 (17)	Sb4^xvi—Ba4—Sb4	84.37 (3)
Sb1ⁱⁱⁱ—Ba1—Sb3	178.223 (18)	In1^xvii—Ba5—In1^xviii	101.39 (2)
Sb2^iv—Ba1—Sb3	94.182 (17)	In1^xvii—Ba5—In1^xix	51.430 (19)
Sb4ⁱ—Ba1—In1ⁱ	89.069 (17)	In1^xviii—Ba5—In1^xix	125.03 (3)
Sb2ⁱⁱ—Ba1—In1ⁱ	90.672 (16)	In1^xvii—Ba5—In1^xx	125.03 (3)
Sb1—Ba1—In1ⁱ	133.506 (16)	In1^xviii—Ba5—In1^xx	51.430 (19)
Sb1ⁱⁱⁱ—Ba1—In1ⁱ	43.815 (13)	In1^xix—Ba5—In1^xx	101.39 (2)
Sb2^iv—Ba1—In1ⁱ	43.967 (12)	In1^xvii—Ba5—Sb1	162.493 (19)
Sb3—Ba1—In1ⁱ	137.062 (18)	In1^xviii—Ba5—Sb1	84.581 (13)
Sb4ⁱ—Ba1—Ba2	125.651 (17)	In1^xix—Ba5—Sb1	111.730 (13)
Sb2ⁱⁱ—Ba1—Ba2	54.554 (13)	In1^xx—Ba5—Sb1	47.322 (13)
Sb1—Ba1—Ba2	50.129 (13)	In1^xvii—Ba5—Sb1ⁱ	47.322 (13)
Sb1ⁱⁱⁱ—Ba1—Ba2	128.386 (16)	In1^xviii—Ba5—Sb1ⁱ	111.730 (13)
Sb2^iv—Ba1—Ba2	131.250 (16)	In1^xix—Ba5—Sb1ⁱ	84.581 (13)
Sb3—Ba1—Ba2	49.885 (14)	In1^xx—Ba5—Sb1ⁱ	162.493 (19)
In1ⁱ—Ba1—Ba2	145.225 (16)	Sb1—Ba5—Sb1ⁱ	145.23 (3)
Sb4ⁱ—Ba1—Ba1ⁱⁱ	47.298 (11)	In1^xvii—Ba5—Sb1^ix	111.730 (13)
Sb2ⁱⁱ—Ba1—Ba1ⁱⁱ	134.518 (11)	In1^xviii—Ba5—Sb1^ix	47.322 (13)
Sb1—Ba1—Ba1ⁱⁱ	91.983 (11)	In1^xix—Ba5—Sb1^ix	162.493 (19)
Sb1ⁱⁱⁱ—Ba1—Ba1ⁱⁱ	131.624 (11)	In1^xx—Ba5—Sb1^ix	84.581 (13)
Sb2^iv—Ba1—Ba1ⁱⁱ	90.267 (10)	Sb1—Ba5—Sb1^ix	84.494 (18)
Sb3—Ba1—Ba1ⁱⁱ	49.790 (10)	Sb1ⁱ—Ba5—Sb1^ix	85.261 (18)
In1ⁱ—Ba1—Ba1ⁱⁱ	123.058 (10)	In1^xvii—Ba5—Sb1ⁱⁱ	84.581 (13)
Ba2—Ba1—Ba1ⁱⁱ	87.579 (9)	In1^xviii—Ba5—Sb1ⁱⁱ	162.493 (19)
Sb4ⁱ—Ba1—Ba1^v	132.64 (2)	In1^xix—Ba5—Sb1ⁱⁱ	47.322 (13)
Sb2ⁱⁱ—Ba1—Ba1^v	48.878 (11)	In1^xx—Ba5—Sb1ⁱⁱ	111.730 (13)
Sb1—Ba1—Ba1^v	131.107 (18)	Sb1—Ba5—Sb1ⁱⁱ	85.261 (18)
Sb1ⁱⁱⁱ—Ba1—Ba1^v	90.449 (16)	Sb1ⁱ—Ba5—Sb1ⁱⁱ	84.494 (18)
Sb2^iv—Ba1—Ba1^v	48.124 (12)	Sb1^ix—Ba5—Sb1ⁱⁱ	145.23 (3)
Sb3—Ba1—Ba1^v	89.306 (16)	In1^xvii—Ba5—Sb3^xii	50.868 (13)
In1ⁱ—Ba1—Ba1^v	57.489 (12)	In1^xviii—Ba5—Sb3^xii	50.868 (13)
Ba2—Ba1—Ba1^v	93.748 (14)	In1^xix—Ba5—Sb3^xii	84.64 (2)
Ba1ⁱⁱ—Ba1—Ba1^v	121.973 (11)	In1^xx—Ba5—Sb3^xii	84.64 (2)
Sb4ⁱ—Ba1—Ba3ⁱ	47.852 (14)	Sb1—Ba5—Sb3^xii	130.627 (17)
Sb2ⁱⁱ—Ba1—Ba3ⁱ	130.506 (15)	Sb1ⁱ—Ba5—Sb3^xii	79.508 (13)
Sb1—Ba1—Ba3ⁱ	48.233 (12)	Sb1^ix—Ba5—Sb3^xii	79.508 (13)
Sb1ⁱⁱⁱ—Ba1—Ba3ⁱ	86.937 (14)	Sb1ⁱⁱ—Ba5—Sb3^xii	130.627 (17)
Sb2^iv—Ba1—Ba3ⁱ	132.382 (15)	In1^xvii—Ba5—Sb3^xxi	84.64 (2)
Sb3—Ba1—Ba3ⁱ	93.283 (15)	In1^xviii—Ba5—Sb3^xxi	84.64 (2)
In1ⁱ—Ba1—Ba3ⁱ	120.632 (14)	In1^xix—Ba5—Sb3^xxi	50.868 (13)
Ba2—Ba1—Ba3ⁱ	87.281 (13)	In1^xx—Ba5—Sb3^xxi	50.868 (13)
Ba1ⁱⁱ—Ba1—Ba3ⁱ	60.565 (7)	Sb1—Ba5—Sb3^xxi	79.508 (13)
Ba1^v—Ba1—Ba3ⁱ	177.275 (17)	Sb1ⁱ—Ba5—Sb3^xxi	130.627 (17)
Sb4ⁱ—Ba1—Ba3^vi	89.567 (16)	Sb1^ix—Ba5—Sb3^xxi	130.627 (17)
Sb2ⁱⁱ—Ba1—Ba3^vi	92.956 (14)	Sb1ⁱⁱ—Ba5—Sb3^xxi	79.508 (13)
Sb1—Ba1—Ba3^vi	135.534 (16)	Sb3^xii—Ba5—Sb3^xxi	76.58 (3)
Sb1ⁱⁱⁱ—Ba1—Ba3^vi	133.841 (15)	In1^xvii—Ba5—Ba2	142.027 (19)
Sb2^iv—Ba1—Ba3^vi	46.886 (12)	In1^xviii—Ba5—Ba2	90.531 (15)
Sb3—Ba1—Ba3^vi	47.337 (14)	In1^xix—Ba5—Ba2	142.027 (19)
In1ⁱ—Ba1—Ba3^vi	90.508 (13)	In1^xx—Ba5—Ba2	90.531 (15)
Ba2—Ba1—Ba3^vi	91.559 (13)	Sb1—Ba5—Ba2	53.194 (13)
Ba1ⁱⁱ—Ba1—Ba3^vi	60.662 (7)	Sb1ⁱ—Ba5—Ba2	94.75 (2)
Ba1^v—Ba1—Ba3^vi	61.312 (12)	Sb1^ix—Ba5—Ba2	53.194 (13)
Ba3ⁱ—Ba1—Ba3^vi	121.212 (11)	Sb1ⁱⁱ—Ba5—Ba2	94.75 (2)
In1^vii—Ba2—In1^viii	51.55 (2)	Sb3^xii—Ba5—Ba2	132.701 (10)
In1^vii—Ba2—In2ⁱⁱ	93.462 (18)	Sb3^xxi—Ba5—Ba2	132.701 (10)
In1^viii—Ba2—In2ⁱⁱ	114.91 (2)	In1^xvii—Ba5—Ba2ⁱ	90.531 (15)
In1^vii—Ba2—In2ⁱ	114.91 (2)	In1^xviii—Ba5—Ba2ⁱ	142.027 (19)
In1^viii—Ba2—In2ⁱ	93.462 (18)	In1^xix—Ba5—Ba2ⁱ	90.531 (15)
In2ⁱⁱ—Ba2—In2ⁱ	49.02 (2)	In1^xx—Ba5—Ba2ⁱ	142.027 (19)
In1^vii—Ba2—Sb1^ix	158.09 (2)	Sb1—Ba5—Ba2ⁱ	94.75 (2)
In1^viii—Ba2—Sb1^ix	109.515 (14)	Sb1ⁱ—Ba5—Ba2ⁱ	53.194 (13)
In2ⁱⁱ—Ba2—Sb1^ix	85.158 (18)	Sb1^ix—Ba5—Ba2ⁱ	94.75 (2)
In2ⁱ—Ba2—Sb1^ix	49.389 (14)	Sb1ⁱⁱ—Ba5—Ba2ⁱ	53.194 (13)
In1^vii—Ba2—Sb1	109.515 (14)	Sb3^xii—Ba5—Ba2ⁱ	132.701 (10)
In1^viii—Ba2—Sb1	158.09 (2)	Sb3^xxi—Ba5—Ba2ⁱ	132.701 (10)
In2ⁱⁱ—Ba2—Sb1	49.389 (14)	Ba2—Ba5—Ba2ⁱ	60.45 (2)
In2ⁱ—Ba2—Sb1	85.158 (18)	Sb1^xxii—In1—Sb2^xv	119.01 (2)
Sb1^ix—Ba2—Sb1	86.12 (2)	Sb1^xxii—In1—In1^xxiii	109.617 (14)
In1^vii—Ba2—Sb3ⁱ	86.49 (2)	Sb2^xv—In1—In1^xxiii	108.387 (14)
In1^viii—Ba2—Sb3ⁱ	51.906 (14)	Sb1^xxii—In1—Sb3^xxiv	104.82 (2)
In2ⁱⁱ—Ba2—Sb3ⁱ	161.643 (18)	Sb2^xv—In1—Sb3^xxiv	109.04 (2)
In2ⁱ—Ba2—Sb3ⁱ	114.761 (14)	In1^xxiii—In1—Sb3^xxiv	105.090 (16)
Sb1^ix—Ba2—Sb3ⁱ	88.083 (16)	Sb1^xxii—In1—Ba2^xxiv	165.95 (2)
Sb1—Ba2—Sb3ⁱ	147.05 (2)	Sb2^xv—In1—Ba2^xxiv	74.947 (19)
In1^vii—Ba2—Sb3	51.906 (14)	In1^xxiii—In1—Ba2^xxiv	64.226 (10)
In1^viii—Ba2—Sb3	86.49 (2)	Sb3^xxiv—In1—Ba2^xxiv	66.660 (19)
In2ⁱⁱ—Ba2—Sb3	114.761 (14)	Sb1^xxii—In1—Ba5^xvii	70.071 (19)
In2ⁱ—Ba2—Sb3	161.643 (18)	Sb2^xv—In1—Ba5^xvii	170.58 (2)
Sb1^ix—Ba2—Sb3	147.05 (2)	In1^xxiii—In1—Ba5^xvii	64.285 (10)
Sb1—Ba2—Sb3	88.083 (16)	Sb3^xxiv—In1—Ba5^xvii	68.962 (19)
Sb3ⁱ—Ba2—Sb3	79.45 (2)	Ba2^xxiv—In1—Ba5^xvii	96.07 (2)
In1^vii—Ba2—Sb2ⁱⁱ	45.739 (13)	Sb1^xxii—In1—Ba1ⁱ	60.226 (15)
In1^viii—Ba2—Sb2ⁱⁱ	80.925 (18)	Sb2^xv—In1—Ba1ⁱ	60.260 (15)
In2ⁱⁱ—Ba2—Sb2ⁱⁱ	47.723 (14)	In1^xxiii—In1—Ba1ⁱ	141.952 (10)
In2ⁱ—Ba2—Sb2ⁱⁱ	80.950 (18)	Sb3^xxiv—In1—Ba1ⁱ	112.95 (2)
Sb1^ix—Ba2—Sb2ⁱⁱ	128.88 (2)	Ba2^xxiv—In1—Ba1ⁱ	132.730 (18)
Sb1—Ba2—Sb2ⁱⁱ	77.265 (13)	Ba5^xvii—In1—Ba1ⁱ	129.15 (2)
Sb3ⁱ—Ba2—Sb2ⁱⁱ	129.50 (2)	Sb4^xxv—In2—In2^ix	111.322 (17)
Sb3—Ba2—Sb2ⁱⁱ	80.918 (14)	Sb4^xxv—In2—Sb1ⁱⁱ	109.93 (2)
In1^vii—Ba2—Sb2ⁱ	80.925 (18)	In2^ix—In2—Sb1ⁱⁱ	110.086 (14)
In1^viii—Ba2—Sb2ⁱ	45.739 (13)	Sb4^xxv—In2—Sb2	113.15 (2)
In2ⁱⁱ—Ba2—Sb2ⁱ	80.950 (18)	In2^ix—In2—Sb2	108.733 (14)
In2ⁱ—Ba2—Sb2ⁱ	47.723 (14)	Sb1ⁱⁱ—In2—Sb2	103.32 (2)
Sb1^ix—Ba2—Sb2ⁱ	77.265 (13)	Sb4^xxv—In2—Ba2ⁱ	173.81 (3)
Sb1—Ba2—Sb2ⁱ	128.88 (2)	In2^ix—In2—Ba2ⁱ	65.488 (10)
Sb3ⁱ—Ba2—Sb2ⁱ	80.918 (14)	Sb1ⁱⁱ—In2—Ba2ⁱ	67.497 (17)
Sb3—Ba2—Sb2ⁱ	129.50 (2)	Sb2—In2—Ba2ⁱ	73.039 (18)
Sb2ⁱⁱ—Ba2—Sb2ⁱ	76.80 (2)	Sb4^xxv—In2—Ba3^xxv	58.068 (19)
In1^vii—Ba2—Ba5	147.398 (15)	In2^ix—In2—Ba3^xxv	140.012 (10)
In1^viii—Ba2—Ba5	147.398 (15)	Sb1ⁱⁱ—In2—Ba3^xxv	109.592 (19)
In2ⁱⁱ—Ba2—Ba5	93.275 (18)	Sb2—In2—Ba3^xxv	56.626 (15)
In2ⁱ—Ba2—Ba5	93.275 (18)	Ba2ⁱ—In2—Ba3^xxv	127.911 (18)
Sb1^ix—Ba2—Ba5	54.396 (13)	In1^xx—Sb1—In2ⁱⁱ	101.88 (2)
Sb1—Ba2—Ba5	54.396 (13)	In1^xx—Sb1—Ba1	161.99 (2)
Sb3ⁱ—Ba2—Ba5	96.619 (17)	In2ⁱⁱ—Sb1—Ba1	85.363 (18)
Sb3—Ba2—Ba5	96.619 (17)	In1^xx—Sb1—Ba1ⁱⁱⁱ	75.959 (17)
Sb2ⁱⁱ—Ba2—Ba5	131.656 (13)	In2ⁱⁱ—Sb1—Ba1ⁱⁱⁱ	79.632 (17)
Sb2ⁱ—Ba2—Ba5	131.656 (13)	Ba1—Sb1—Ba1ⁱⁱⁱ	89.375 (16)
In1^vii—Ba2—Ba2ⁱ	98.579 (14)	In1^xx—Sb1—Ba3ⁱ	84.155 (19)
In1^viii—Ba2—Ba2ⁱ	98.579 (14)	In2ⁱⁱ—Sb1—Ba3ⁱ	161.77 (2)
In2ⁱⁱ—Ba2—Ba2ⁱ	144.428 (13)	Ba1—Sb1—Ba3ⁱ	84.272 (16)
In2ⁱ—Ba2—Ba2ⁱ	144.428 (13)	Ba1ⁱⁱⁱ—Sb1—Ba3ⁱ	85.293 (16)
Sb1^ix—Ba2—Ba2ⁱ	95.073 (13)	In1^xx—Sb1—Ba2	117.27 (2)
Sb1—Ba2—Ba2ⁱ	95.073 (13)	In2ⁱⁱ—Sb1—Ba2	63.114 (17)
Sb3ⁱ—Ba2—Ba2ⁱ	53.198 (11)	Ba1—Sb1—Ba2	80.729 (16)
Sb3—Ba2—Ba2ⁱ	53.198 (11)	Ba1ⁱⁱⁱ—Sb1—Ba2	141.977 (19)
Sb2ⁱⁱ—Ba2—Ba2ⁱ	133.895 (11)	Ba3ⁱ—Sb1—Ba2	129.426 (19)
Sb2ⁱ—Ba2—Ba2ⁱ	133.895 (11)	In1^xx—Sb1—Ba5	62.606 (19)
Ba5—Ba2—Ba2ⁱ	59.775 (11)	In2ⁱⁱ—Sb1—Ba5	117.648 (19)
Sb2^x—Ba3—Sb2^xi	84.66 (2)	Ba1—Sb1—Ba5	128.543 (19)
Sb2^x—Ba3—Sb3^xii	97.024 (18)	Ba1ⁱⁱⁱ—Sb1—Ba5	137.18 (2)
Sb2^xi—Ba3—Sb3^xii	97.024 (18)	Ba3ⁱ—Sb1—Ba5	80.461 (15)
Sb2^x—Ba3—Sb4	86.702 (17)	Ba2—Sb1—Ba5	72.411 (18)
Sb2^xi—Ba3—Sb4	86.702 (17)	In1^xxvi—Sb2—In2	118.55 (2)
Sb3^xii—Ba3—Sb4	174.94 (2)	In1^xxvi—Sb2—Ba3^xxv	158.88 (2)
Sb2^x—Ba3—Sb1^ix	178.605 (18)	In2—Sb2—Ba3^xxv	78.130 (18)
Sb2^xi—Ba3—Sb1^ix	94.053 (13)	In1^xxvi—Sb2—Ba1ⁱⁱ	82.178 (18)
Sb3^xii—Ba3—Sb1^ix	82.585 (17)	In2—Sb2—Ba1ⁱⁱ	84.879 (18)
Sb4—Ba3—Sb1^ix	93.769 (17)	Ba3^xxv—Sb2—Ba1ⁱⁱ	86.909 (16)
Sb2^x—Ba3—Sb1ⁱ	94.053 (13)	In1^xxvi—Sb2—Ba1^xxvii	75.772 (18)
Sb2^xi—Ba3—Sb1ⁱ	178.605 (18)	In2—Sb2—Ba1^xxvii	159.71 (2)
Sb3^xii—Ba3—Sb1ⁱ	82.585 (17)	Ba3^xxv—Sb2—Ba1^xxvii	85.014 (17)
Sb4—Ba3—Sb1ⁱ	93.769 (17)	Ba1ⁱⁱ—Sb2—Ba1^xxvii	82.998 (15)
Sb1^ix—Ba3—Sb1ⁱ	87.23 (2)	In1^xxvi—Sb2—Ba4^xiv	93.71 (2)
Sb2^x—Ba3—In2^x	45.244 (13)	In2—Sb2—Ba4^xiv	96.72 (2)
Sb2^xi—Ba3—In2^x	91.297 (18)	Ba3^xxv—Sb2—Ba4^xiv	97.149 (16)
Sb3^xii—Ba3—In2^x	140.454 (14)	Ba1ⁱⁱ—Sb2—Ba4^xiv	175.863 (18)
Sb4—Ba3—In2^x	42.412 (12)	Ba1^xxvii—Sb2—Ba4^xiv	96.509 (19)
Sb1^ix—Ba3—In2^x	135.44 (2)	In1^xxvi—Sb2—Ba2ⁱ	59.314 (17)
Sb1ⁱ—Ba3—In2^x	88.172 (14)	In2—Sb2—Ba2ⁱ	59.238 (16)
Sb2^x—Ba3—In2^xi	91.297 (18)	Ba3^xxv—Sb2—Ba2ⁱ	135.28 (2)
Sb2^xi—Ba3—In2^xi	45.244 (13)	Ba1ⁱⁱ—Sb2—Ba2ⁱ	77.125 (15)
Sb3^xii—Ba3—In2^xi	140.454 (14)	Ba1^xxvii—Sb2—Ba2ⁱ	132.629 (18)
Sb4—Ba3—In2^xi	42.412 (12)	Ba4^xiv—Sb2—Ba2ⁱ	100.382 (15)
Sb1^ix—Ba3—In2^xi	88.172 (14)	In1^vii—Sb3—In1^xxvi	119.85 (3)
Sb1ⁱ—Ba3—In2^xi	135.44 (2)	In1^vii—Sb3—Ba3^vi	81.640 (18)
In2^x—Ba3—In2^xi	65.310 (18)	In1^xxvi—Sb3—Ba3^vi	81.641 (18)
Sb2^x—Ba3—Ba5	130.270 (14)	In1^vii—Sb3—Ba2ⁱ	123.96 (2)
Sb2^xi—Ba3—Ba5	130.270 (14)	In1^xxvi—Sb3—Ba2ⁱ	61.434 (16)
Sb3^xii—Ba3—Ba5	51.447 (18)	Ba3^vi—Sb3—Ba2ⁱ	141.785 (14)
Sb4—Ba3—Ba5	123.49 (2)	In1^vii—Sb3—Ba2	61.434 (16)
Sb1^ix—Ba3—Ba5	50.390 (12)	In1^xxvi—Sb3—Ba2	123.96 (2)
Sb1ⁱ—Ba3—Ba5	50.390 (12)	Ba3^vi—Sb3—Ba2	141.785 (14)
In2^x—Ba3—Ba5	138.151 (14)	Ba2ⁱ—Sb3—Ba2	73.60 (2)
In2^xi—Ba3—Ba5	138.151 (14)	In1^vii—Sb3—Ba1	77.750 (14)
Sb2^x—Ba3—Ba1^ix	132.982 (18)	In1^xxvi—Sb3—Ba1	154.85 (2)
Sb2^xi—Ba3—Ba1^ix	91.140 (13)	Ba3^vi—Sb3—Ba1	83.695 (17)
Sb3^xii—Ba3—Ba1^ix	129.919 (16)	Ba2ⁱ—Sb3—Ba1	126.13 (2)
Sb4—Ba3—Ba1^ix	46.281 (12)	Ba2—Sb3—Ba1	79.407 (14)
Sb1^ix—Ba3—Ba1^ix	47.495 (11)	In1^vii—Sb3—Ba1ⁱⁱ	154.85 (2)
Sb1ⁱ—Ba3—Ba1^ix	90.133 (16)	In1^xxvi—Sb3—Ba1ⁱⁱ	77.750 (14)
In2^x—Ba3—Ba1^ix	88.244 (15)	Ba3^vi—Sb3—Ba1ⁱⁱ	83.695 (17)
In2^xi—Ba3—Ba1^ix	55.877 (11)	Ba2ⁱ—Sb3—Ba1ⁱⁱ	79.407 (14)
Ba5—Ba3—Ba1^ix	86.529 (14)	Ba2—Sb3—Ba1ⁱⁱ	126.13 (2)
Sb2^x—Ba3—Ba1ⁱ	91.140 (13)	Ba1—Sb3—Ba1ⁱⁱ	80.42 (2)
Sb2^xi—Ba3—Ba1ⁱ	132.982 (18)	In1^vii—Sb3—Ba5^xxviii	60.170 (15)
Sb3^xii—Ba3—Ba1ⁱ	129.919 (16)	In1^xxvi—Sb3—Ba5^xxviii	60.170 (15)
Sb4—Ba3—Ba1ⁱ	46.281 (12)	Ba3^vi—Sb3—Ba5^xxviii	80.13 (2)
Sb1^ix—Ba3—Ba1ⁱ	90.133 (16)	Ba2ⁱ—Sb3—Ba5^xxviii	89.005 (18)
Sb1ⁱ—Ba3—Ba1ⁱ	47.495 (11)	Ba2—Sb3—Ba5^xxviii	89.005 (18)
In2^x—Ba3—Ba1ⁱ	55.877 (11)	Ba1—Sb3—Ba5^xxviii	136.530 (13)
In2^xi—Ba3—Ba1ⁱ	88.244 (15)	Ba1ⁱⁱ—Sb3—Ba5^xxviii	136.530 (13)
Ba5—Ba3—Ba1ⁱ	86.529 (14)	In2^x—Sb4—In2^xi	103.75 (3)
Ba1^ix—Ba3—Ba1ⁱ	58.870 (14)	In2^x—Sb4—Ba1^ix	162.15 (3)
Sb2^x—Ba3—Ba1^xii	48.100 (12)	In2^xi—Sb4—Ba1^ix	83.388 (15)
Sb2^xi—Ba3—Ba1^xii	89.545 (17)	In2^x—Sb4—Ba1ⁱ	83.388 (15)
Sb3^xii—Ba3—Ba1^xii	48.968 (13)	In2^xi—Sb4—Ba1ⁱ	162.15 (3)
Sb4—Ba3—Ba1^xii	134.789 (16)	Ba1^ix—Sb4—Ba1ⁱ	85.40 (2)
Sb1^ix—Ba3—Ba1^xii	131.442 (18)	In2^x—Sb4—Ba3	79.52 (2)
Sb1ⁱ—Ba3—Ba1^xii	89.193 (13)	In2^xi—Sb4—Ba3	79.52 (2)
In2^x—Ba3—Ba1^xii	92.751 (13)	Ba1^ix—Sb4—Ba3	85.867 (17)
In2^xi—Ba3—Ba1^xii	125.221 (17)	Ba1ⁱ—Sb4—Ba3	85.867 (17)
Ba5—Ba3—Ba1^xii	92.258 (15)	In2^x—Sb4—Ba4	97.21 (2)
Ba1^ix—Ba3—Ba1^xii	178.779 (18)	In2^xi—Sb4—Ba4	97.21 (2)
Ba1ⁱ—Ba3—Ba1^xii	121.212 (11)	Ba1^ix—Sb4—Ba4	98.083 (19)
Sb2^xiii—Ba4—Sb2^xiv	135.28 (3)	Ba1ⁱ—Sb4—Ba4	98.083 (19)
Sb2^xiii—Ba4—Sb2^viii	82.364 (19)	Ba3—Sb4—Ba4	174.60 (3)

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

Experimental details

Crystal data
Chemical formula	Ba₅In₄Sb₆
M_r	1876.48
Crystal system, space group	Orthorhombic, Pmmn
Temperature (K)	120
a, b, c (Å)	14.2723 (13), 18.3578 (17), 8.2710 (8)
V (Å³)	2167.1 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	20.39
Crystal size (mm)	0.06 × 0.03 × 0.02

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2005)
T_min, T_max	0.374, 0.686
No. of measured, independent and observed [I > 2σ(I)] reflections	12962, 2676, 2098
R_int	0.050
(sin θ/λ)_max (Å⁻¹)	0.651

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.055, 1.02
No. of reflections	2676
No. of parameters	79
Δρ_max, Δρ_min (e Å⁻³)	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

Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
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Iandelli, A. (1964). Z. Anorg. Allg. Chem. 330, 221–232. CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar