Zn(2)(TeO(3))Br(2).

Single crystals of dizinc tellurium dibromide trioxide, Zn(2)(TeO(3))Br(2), were synthesized via a transport reaction in sealed evacuated silica tubes. The compound has a layered crystal structure in which the building units are [ZnO(4)Br] distorted square pyramids, [ZnO(2)Br(2)] distorted tetra-hedra, and [TeO(3)E] tetra-hedra (E being the 5s(2) lone pair of Te(4+)) joined through sharing of edges and corners to form layers of no net charge. Bromine atoms and tellurium lone pairs protrude from the surfaces of each layer towards adjacent layers. This new compound Zn(2)(TeO(3))Br(2) is isostructural with the synthetic compounds Zn(2)(TeO(3))Cl(2), CuZn(TeO(3))(2), Co(2)(TeO(3))Br(2) and the mineral sophiite, Zn(2)(SeO(3))Cl(2).

Related literature

For related literature, see: Becker et al. (2006 ▶); Johnsson & Törnroos (2003a ▶,b ▶, 2007 ▶); Semenova et al. (1992 ▶); Brown & Altermatt (1985 ▶); Galy et al. (1975 ▶).

Experimental

Crystal data

Zn2(TeO3)Br2

M = 466.18

Orthorhombic,

a = 10.5446 (2) Å

b = 16.0928 (2) Å

c = 7.7242 (1) Å

V = 1310.74 (3) Å3

Z = 8

Mo Kα radiation

μ = 23.79 mm−1

T = 293 (2) K

0.20 × 0.16 × 0.04 mm

Data collection

Oxford Diffraction Xcalibur3diffractometer

Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2007); T min = 0.05, T max = 0.35

15561 measured reflections

1290 independent reflections

1201 reflections with I > 2σ(I)

R int = 0.026

Refinement

R[F 2 > 2σ(F 2)] = 0.022

wR(F 2) = 0.055

S = 1.09

1290 reflections

74 parameters

Δρmax = 1.08 e Å−3

Δρmin = −0.82 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Bergerhoff, 1996 ▶); software used to prepare material for publication: enCIFer (Allen et al., 2004 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808011252/pk2093sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808011252/pk2093Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Zn2(TeO3)Br2	F(000) = 1648
Mr = 466.18	Dx = 4.725 Mg m−3
Orthorhombic, Pccn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ab 2ac	Cell parameters from 13770 reflections
a = 10.5446 (2) Å	θ = 3.7–33.2°
b = 16.0928 (2) Å	µ = 23.79 mm−1
c = 7.7242 (1) Å	T = 293 K
V = 1310.74 (3) Å3	Block, colourless
Z = 8	0.21 × 0.16 × 0.04 mm

Oxford Diffraction Xcalibur3 diffractometer	1290 independent reflections
Radiation source: fine-focus sealed tube	1201 reflections with I > 2σ(I)
graphite	Rint = 0.026
φ and ω scans	θmax = 26.3°, θmin = 4.1°
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2007)	h = −12→12
Tmin = 0.05, Tmax = 0.35	k = −20→20
15561 measured reflections	l = −9→9

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)] = 0.022	w = 1/[σ2(Fo2) + (0.0333P)2 + 5.0559P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055	(Δ/σ)max = 0.001
S = 1.09	Δρmax = 1.08 e Å−3
1290 reflections	Δρmin = −0.82 e Å−3
74 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraints	Extinction coefficient: 0.00342 (15)

Experimental. a multifaceted crystal model based on expressions derived by Clark & Reid (1995)]

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	Uiso*/Ueq
Te	0.02983 (3)	0.592957 (18)	0.21187 (3)	0.01207 (12)
Zn1	−0.00948 (6)	0.39234 (4)	0.34333 (7)	0.01639 (15)
Zn2	0.26526 (5)	0.52410 (4)	0.39968 (7)	0.01671 (16)
Br2	0.20748 (5)	0.37261 (3)	0.43887 (7)	0.02286 (16)
Br1	−0.08838 (7)	0.29014 (3)	0.15586 (7)	0.03163 (18)
O2	0.1882 (3)	0.5524 (2)	0.1440 (4)	0.0160 (7)
O1	−0.0568 (3)	0.4903 (2)	0.1969 (4)	0.0155 (7)
O3	0.0906 (3)	0.5786 (2)	0.4378 (4)	0.0158 (7)

	U11	U22	U33	U12	U13	U23
Te	0.0105 (2)	0.01301 (18)	0.01267 (17)	0.00006 (11)	−0.00162 (10)	0.00168 (10)
Zn1	0.0188 (3)	0.0174 (3)	0.0130 (3)	0.0018 (2)	0.0002 (2)	−0.0011 (2)
Zn2	0.0110 (3)	0.0260 (3)	0.0132 (3)	0.0033 (2)	−0.0005 (2)	−0.0016 (2)
Br2	0.0163 (3)	0.0204 (3)	0.0318 (3)	0.0013 (2)	−0.00128 (19)	0.00377 (19)
Br1	0.0530 (4)	0.0191 (3)	0.0227 (3)	−0.0070 (3)	−0.0101 (2)	−0.0017 (2)
O2	0.0094 (17)	0.0266 (19)	0.0120 (14)	0.0012 (14)	0.0001 (12)	−0.0007 (13)
O1	0.0125 (18)	0.0165 (16)	0.0174 (15)	−0.0034 (14)	−0.0037 (13)	0.0013 (13)
O3	0.0138 (18)	0.0230 (18)	0.0105 (15)	0.0024 (15)	−0.0023 (12)	−0.0016 (12)

Te—O2	1.867 (3)	Zn1—Br2	2.4247 (8)
Te—O3	1.873 (3)	Zn2—O2ii	2.002 (3)
Te—O1	1.891 (3)	Zn2—O1iii	2.033 (3)
Zn1—O3i	1.952 (3)	Zn2—O3	2.061 (3)
Zn1—O1	2.004 (3)	Zn2—O2	2.184 (3)
Zn1—Br1	2.3438 (8)	Zn2—Br2	2.5310 (8)
O2—Te—O3	85.00 (14)	O2ii—Zn2—O3	89.30 (13)
O2—Te—O1	96.31 (15)	O1iii—Zn2—O3	157.82 (14)
O3—Te—O1	96.55 (14)	O2ii—Zn2—O2	153.62 (18)
O3i—Zn1—O1	101.01 (14)	O1iii—Zn2—O2	92.03 (12)
O3i—Zn1—Br1	123.23 (11)	O3—Zn2—O2	73.00 (12)
O1—Zn1—Br1	96.62 (10)	O2ii—Zn2—Br2	99.54 (10)
O3i—Zn1—Br2	100.43 (10)	O1iii—Zn2—Br2	98.97 (10)
O1—Zn1—Br2	120.65 (10)	O3—Zn2—Br2	100.22 (10)
Br1—Zn1—Br2	115.54 (3)	O2—Zn2—Br2	102.69 (10)
O2ii—Zn2—O1iii	98.37 (13)