Literature DB >> 23723748

Ba2Sb4GeS10.

Abstract

The title quaternary compound, dibarium tetra-anti-mony germanium deca-sulfide, Ba2Sb4GeS10, crystallizes in a novel three-dimensional ∞ (3)[Sb4GeS10](4-) network structure, which is composed of triangular pyramidal SbS3 (site symmetry m..), distorted SbS5 (m..) polyhedra and regular GeS4 (-4..) tetra-hedra. The SbS3 and SbS5 units are connected with each other through corner- and edge-sharing, forming a Sb4S10 layer in the ab plane. The GeS4 tetra-hedra further bridge two neighbouring Sb4S10 layers, forming a three-dimensional ∞ (3)[Sb4GeS10](4-) network. The Ba(2+) cation (..2) is located between two Sb4S10 layers and is coordinated by ten S atoms with Ba-S bond lengths in the range 3.2505 (9)-3.4121 (2) Å.

Entities: Chemical Disease Gene Species

Year: 2013 PMID： 23723748 PMCID： PMC3647782 DOI： 10.1107/S1600536813007988

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

The stereochemically active 5s 2 lone-pair electrons possess a large electric dipole moment and can influence structures that contain Sb3+, see: Choi & Kanatzidis (2000 ▶); Babo & Albrecht-Schmitt (2012 ▶). SbS3, SbS4 or SbS5 units in a crystal structure are prone to form Sb—S chains through corner- or edge-sharing, see: Dorrscheidt & Schäfer (1981 ▶); Cordier et al. (1984 ▶). GeS4 tetrahedra can be utilized as the second structural unit and introduced into crystal structures to connect Sb—S chains into a two-dimensional layer or three-dimensional framework structure (Feng et al., 2008 ▶). For crystal structures and optical properties, see: Deng et al. (2005 ▶); Kim et al. (2008 ▶); Ribes et al. (1973 ▶); Teske (1979 ▶); Lekse et al. (2009 ▶).

Experimental

Crystal data

Ba2Sb4GeS10 M = 1154.87 Tetragonal, a = 11.3119 (4) Å c = 13.6384 (9) Å V = 1745.16 (14) Å3 Z = 4 Mo Kα radiation μ = 13.40 mm−1 T = 293 K 0.22 × 0.07 × 0.07 mm

Data collection

Rigaku SCXMini CCD diffractometer Absorption correction: multi-scan (CrystalClear; Rigaku, 2007 ▶) T min = 0.530, T max = 1.000 12411 measured reflections 1046 independent reflections 1032 reflections with I > 2σ(I) R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.018 wR(F 2) = 0.042 S = 1.15 1046 reflections 45 parameters Δρmax = 0.66 e Å−3 Δρmin = −0.74 e Å−3 Data collection: CrystalClear (Rigaku, 2007 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2005 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Click here for additional data file. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813007988/jj2163sup1.cif Click here for additional data file. Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813007988/jj2163Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Ba₂Sb₄GeS₁₀	D_x = 4.395 Mg m⁻³
M_r = 1154.87	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4₂/mbc	Cell parameters from 1877 reflections
Hall symbol: -P 4ac 2ab	θ = 2.3–27.5°
a = 11.3119 (4) Å	µ = 13.40 mm⁻¹
c = 13.6384 (9) Å	T = 293 K
V = 1745.16 (14) Å³	Rod, dark-red
Z = 4	0.22 × 0.07 × 0.07 mm
F(000) = 2032

Rigaku SCXMini CCD diffractometer	1046 independent reflections
Radiation source: fine-focus sealed tube	1032 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.030
CCD_Profile_fitting scans	θ_max = 27.5°, θ_min = 2.6°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2007)	h = −14→14
T_min = 0.530, T_max = 1.000	k = −14→11
12411 measured reflections	l = −16→17

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)] = 0.018	w = 1/[σ²(F_o²) + (0.0214P)² + 3.2912P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.042	(Δ/σ)_max < 0.001
S = 1.15	Δρ_max = 0.66 e Å⁻³
1046 reflections	Δρ_min = −0.74 e Å⁻³
45 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00225 (8)

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.

	x	y	z	U_iso*/U_eq
Ba1	0.232424 (19)	0.732424 (19)	0.2500	0.01704 (10)
Sb1	0.13578 (3)	0.41567 (3)	0.0000	0.01543 (10)
Sb2	0.46488 (3)	0.34169 (3)	0.0000	0.01796 (10)
Ge1	0.0000	0.0000	0.2500	0.01175 (15)
S1	0.27060 (10)	0.24355 (10)	0.0000	0.0136 (2)
S2	0.01781 (8)	0.15428 (7)	0.34843 (6)	0.01631 (18)
S3	0.02261 (7)	0.32137 (8)	0.13186 (6)	0.01777 (19)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ba1	0.01715 (12)	0.01715 (12)	0.01683 (15)	0.00214 (11)	−0.00097 (7)	0.00097 (7)
Sb1	0.01518 (17)	0.01341 (17)	0.01771 (17)	0.00143 (11)	0.000	0.000
Sb2	0.01151 (17)	0.02030 (18)	0.02206 (18)	−0.00225 (12)	0.000	0.000
Ge1	0.0126 (2)	0.0126 (2)	0.0101 (3)	0.000	0.000	0.000
S1	0.0101 (5)	0.0121 (5)	0.0184 (6)	−0.0006 (4)	0.000	0.000
S2	0.0201 (4)	0.0142 (4)	0.0146 (4)	−0.0020 (3)	−0.0009 (3)	−0.0026 (3)
S3	0.0131 (4)	0.0254 (4)	0.0147 (4)	−0.0025 (3)	0.0024 (3)	−0.0028 (3)

Ba1—S2ⁱ	3.2505 (9)	Sb2—S3^viii	2.6576 (9)
Ba1—S2ⁱⁱ	3.2505 (9)	Sb2—S2^iv	2.9352 (9)
Ba1—S3ⁱⁱ	3.3596 (9)	Sb2—S2^ix	2.9352 (9)
Ba1—S3ⁱ	3.3596 (9)	Ge1—S2	2.2110 (8)
Ba1—S3ⁱⁱⁱ	3.3599 (8)	Ge1—S2^x	2.2110 (8)
Ba1—S3^iv	3.3599 (8)	Ge1—S2^xi	2.2110 (8)
Ba1—S2^iv	3.3849 (9)	Ge1—S2^xii	2.2110 (8)
Ba1—S2ⁱⁱⁱ	3.3849 (9)	S1—Ba1^xiii	3.4121 (2)
Ba1—S1ⁱⁱ	3.4121 (2)	S1—Ba1^xiv	3.4121 (2)
Ba1—S1^v	3.4121 (2)	S2—Sb2^xv	2.9352 (9)
Sb1—S3^vi	2.4517 (9)	S2—Ba1^xiv	3.2505 (9)
Sb1—S3	2.4517 (9)	S2—Ba1ⁱⁱⁱ	3.3849 (9)
Sb1—S1	2.4732 (12)	S3—Sb2^xvi	2.6576 (9)
Sb2—S1	2.4621 (12)	S3—Ba1^xiv	3.3596 (9)
Sb2—S3^vii	2.6576 (9)	S3—Ba1ⁱⁱⁱ	3.3599 (8)

S2ⁱ—Ba1—S2ⁱⁱ	130.04 (3)	S3^iv—Ba1—S1^v	120.60 (3)
S2ⁱ—Ba1—S3ⁱⁱ	76.46 (2)	S2^iv—Ba1—S1^v	68.80 (2)
S2ⁱⁱ—Ba1—S3ⁱⁱ	64.06 (2)	S2ⁱⁱⁱ—Ba1—S1^v	111.96 (2)
S2ⁱ—Ba1—S3ⁱ	64.06 (2)	S1ⁱⁱ—Ba1—S1^v	177.82 (4)
S2ⁱⁱ—Ba1—S3ⁱ	76.46 (2)	S3^vi—Sb1—S3	94.37 (4)
S3ⁱⁱ—Ba1—S3ⁱ	74.69 (3)	S3^vi—Sb1—S1	88.82 (3)
S2ⁱ—Ba1—S3ⁱⁱⁱ	153.52 (2)	S3—Sb1—S1	88.82 (3)
S2ⁱⁱ—Ba1—S3ⁱⁱⁱ	74.09 (2)	S1—Sb2—S3^vii	84.63 (3)
S3ⁱⁱ—Ba1—S3ⁱⁱⁱ	129.53 (3)	S1—Sb2—S3^viii	84.63 (3)
S3ⁱ—Ba1—S3ⁱⁱⁱ	122.17 (3)	S3^vii—Sb2—S3^viii	85.17 (4)
S2ⁱ—Ba1—S3^iv	74.09 (2)	S1—Sb2—S2^iv	80.46 (3)
S2ⁱⁱ—Ba1—S3^iv	153.52 (2)	S3^vii—Sb2—S2^iv	164.84 (3)
S3ⁱⁱ—Ba1—S3^iv	122.17 (3)	S3^viii—Sb2—S2^iv	90.69 (3)
S3ⁱ—Ba1—S3^iv	129.53 (3)	S1—Sb2—S2^ix	80.46 (3)
S3ⁱⁱⁱ—Ba1—S3^iv	85.35 (3)	S3^vii—Sb2—S2^ix	90.69 (3)
S2ⁱ—Ba1—S2^iv	66.88 (3)	S3^viii—Sb2—S2^ix	164.84 (3)
S2ⁱⁱ—Ba1—S2^iv	131.76 (3)	S2^iv—Sb2—S2^ix	89.54 (3)
S3ⁱⁱ—Ba1—S2^iv	140.05 (2)	S2—Ge1—S2^x	111.63 (2)
S3ⁱ—Ba1—S2^iv	75.40 (2)	S2—Ge1—S2^xi	105.23 (4)
S3ⁱⁱⁱ—Ba1—S2^iv	89.05 (2)	S2^x—Ge1—S2^xi	111.63 (2)
S3^iv—Ba1—S2^iv	62.66 (2)	S2—Ge1—S2^xii	111.63 (2)
S2ⁱ—Ba1—S2ⁱⁱⁱ	131.76 (3)	S2^x—Ge1—S2^xii	105.23 (4)
S2ⁱⁱ—Ba1—S2ⁱⁱⁱ	66.88 (3)	S2^xi—Ge1—S2^xii	111.63 (2)
S3ⁱⁱ—Ba1—S2ⁱⁱⁱ	75.40 (2)	Sb2—S1—Sb1	101.27 (4)
S3ⁱ—Ba1—S2ⁱⁱⁱ	140.05 (2)	Sb2—S1—Ba1^xiii	91.466 (19)
S3ⁱⁱⁱ—Ba1—S2ⁱⁱⁱ	62.66 (2)	Sb1—S1—Ba1^xiii	91.31 (2)
S3^iv—Ba1—S2ⁱⁱⁱ	89.05 (2)	Sb2—S1—Ba1^xiv	91.466 (19)
S2^iv—Ba1—S2ⁱⁱⁱ	142.24 (3)	Sb1—S1—Ba1^xiv	91.31 (2)
S2ⁱ—Ba1—S1ⁱⁱ	63.42 (2)	Ba1^xiii—S1—Ba1^xiv	175.62 (4)
S2ⁱⁱ—Ba1—S1ⁱⁱ	115.56 (2)	Ge1—S2—Sb2^xv	96.58 (3)
S3ⁱⁱ—Ba1—S1ⁱⁱ	61.18 (2)	Ge1—S2—Ba1^xiv	92.47 (3)
S3ⁱ—Ba1—S1ⁱⁱ	116.86 (3)	Sb2^xv—S2—Ba1^xiv	86.85 (2)
S3ⁱⁱⁱ—Ba1—S1ⁱⁱ	120.60 (3)	Ge1—S2—Ba1ⁱⁱⁱ	88.96 (3)
S3^iv—Ba1—S1ⁱⁱ	61.24 (2)	Sb2^xv—S2—Ba1ⁱⁱⁱ	154.96 (3)
S2^iv—Ba1—S1ⁱⁱ	111.96 (2)	Ba1^xiv—S2—Ba1ⁱⁱⁱ	117.39 (2)
S2ⁱⁱⁱ—Ba1—S1ⁱⁱ	68.80 (2)	Sb1—S3—Sb2^xvi	86.21 (3)
S2ⁱ—Ba1—S1^v	115.56 (2)	Sb1—S3—Ba1^xiv	92.95 (3)
S2ⁱⁱ—Ba1—S1^v	63.42 (2)	Sb2^xvi—S3—Ba1^xiv	108.63 (3)
S3ⁱⁱ—Ba1—S1^v	116.86 (3)	Sb1—S3—Ba1ⁱⁱⁱ	151.51 (4)
S3ⁱ—Ba1—S1^v	61.18 (2)	Sb2^xvi—S3—Ba1ⁱⁱⁱ	89.30 (2)
S3ⁱⁱⁱ—Ba1—S1^v	61.24 (2)	Ba1^xiv—S3—Ba1ⁱⁱⁱ	115.09 (3)

S3^vii—Sb2—S1—Sb1	−137.18 (2)	S3—Sb1—S1—Ba1^xiv	−41.05 (3)
S3^viii—Sb2—S1—Sb1	137.18 (2)	S2^x—Ge1—S2—Sb2^xv	157.74 (2)
S2^iv—Sb2—S1—Sb1	45.572 (18)	S2^xi—Ge1—S2—Sb2^xv	36.474 (13)
S2^ix—Sb2—S1—Sb1	−45.572 (18)	S2^xii—Ge1—S2—Sb2^xv	−84.791 (7)
S3^vii—Sb2—S1—Ba1^xiii	−45.55 (3)	S2^x—Ge1—S2—Ba1^xiv	−115.15 (4)
S3^viii—Sb2—S1—Ba1^xiii	−131.19 (3)	S2^xi—Ge1—S2—Ba1^xiv	123.59 (3)
S2^iv—Sb2—S1—Ba1^xiii	137.20 (3)	S2^xii—Ge1—S2—Ba1^xiv	2.32 (3)
S2^ix—Sb2—S1—Ba1^xiii	46.06 (2)	S2^x—Ge1—S2—Ba1ⁱⁱⁱ	2.23 (2)
S3^vii—Sb2—S1—Ba1^xiv	131.19 (3)	S2^xi—Ge1—S2—Ba1ⁱⁱⁱ	−119.04 (3)
S3^viii—Sb2—S1—Ba1^xiv	45.55 (3)	S2^xii—Ge1—S2—Ba1ⁱⁱⁱ	119.70 (3)
S2^iv—Sb2—S1—Ba1^xiv	−46.06 (2)	S3^vi—Sb1—S3—Sb2^xvi	22.13 (4)
S2^ix—Sb2—S1—Ba1^xiv	−137.20 (3)	S1—Sb1—S3—Sb2^xvi	−66.60 (3)
S3^vi—Sb1—S1—Sb2	132.80 (2)	S3^vi—Sb1—S3—Ba1^xiv	130.615 (18)
S3—Sb1—S1—Sb2	−132.80 (2)	S1—Sb1—S3—Ba1^xiv	41.89 (3)
S3^vi—Sb1—S1—Ba1^xiii	41.05 (3)	S3^vi—Sb1—S3—Ba1ⁱⁱⁱ	−59.38 (9)
S3—Sb1—S1—Ba1^xiii	135.44 (3)	S1—Sb1—S3—Ba1ⁱⁱⁱ	−148.11 (7)
S3^vi—Sb1—S1—Ba1^xiv	−135.44 (3)

4 in total

1. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

2. Three-dimensional chiral microporous germanium antimony sulfide with ion-exchange properties.

Authors: Mei-Ling Feng; De-Nian Kong; Zai-Lai Xie; Xiao-Ying Huang
Journal: Angew Chem Int Ed Engl Date: 2008 Impact factor: 15.336

3. Sulfosalts with alkaline earth metals. Centrosymmetric vs acentric interplay in Ba3Sb4.66S10 and Ba2.62Pb1.38Sb4S10 based on the Ba/Pb/Sb ratio. Phases related to arsenosulfide minerals of the rathite group and the novel polysulfide Sr6Sb6S17.

Authors: K S Choi; M G Kanatzidis
Journal: Inorg Chem Date: 2000-12-11 Impact factor: 5.165

4. Second-harmonic generation and crystal structure of the diamond-like semiconductors Li(2)CdGeS(4) and Li(2)CdSnS(4).

Authors: Jonathan W Lekse; Meghann A Moreau; Katie L McNerny; Jeongho Yeon; P Shiv Halasyamani; Jennifer A Aitken
Journal: Inorg Chem Date: 2009-08-17 Impact factor: 5.165

4 in total