Hexaaqua-dibromidoeuropium(III) bromide, [EuBr(2)(H(2)O)(6)]Br.

The title compound crystallizes with the GdCl(3)·6H(2)O structure type, exhibiting discrete [EuBr(2)(H(2)O)(6)](+) cations as the main building blocks, linked with isolated bromide anions via H⋯Br hydrogen bonds to form a complex framework. The Eu atom and one Br atom each lie on a twofold rotation axis.

Related literature

For related literature, see: Bärnighausen et al. (1965 ▶); Bell & Smith (1990 ▶); Burns & Peterson (1971 ▶); Demyanets et al. (1974 ▶); Duhlev et al. (1988 ▶); Graeber et al. (1966 ▶); Habenschuss & Spedding (1980 ▶); Junk et al. (1999 ▶); Kolitsch (2006 ▶); Marezio et al. (1961 ▶); Reuter et al. (1994 ▶); Tegenfeldt et al. (1979 ▶); Wickleder & Meyer (1995 ▶).

Experimental

Crystal data

[EuBr2(H2O)6]Br

M = 499.79

Monoclinic,

a = 8.1672 (7) Å

b = 6.7538 (4) Å

c = 12.5451 (10) Å

β = 127.077 (5)°

V = 552.08 (8) Å3

Z = 2

Mo Kα radiation

μ = 16.52 mm−1

T = 293 (2) K

0.25 × 0.24 × 0.18 mm

Data collection

Stoe IPDSII diffractometer

Absorption correction: numerical [X-RED (Stoe & Cie, 2001 ▶) and X-SHAPE (Stoe & Cie, 1999 ▶)] T min = 0.065, T max = 0.155

10921 measured reflections

1613 independent reflections

1397 reflections with I > 2s(I)

R int = 0.067

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.049

S = 1.11

1613 reflections

72 parameters

All H-atom parameters refined

Δρmax = 1.14 e Å−3

Δρmin = −1.10 e Å−3

Data collection: X-AREA (Stoe & Cie, 2006 ▶); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DRAWXTL (Finger et al., 2007 ▶); software used to prepare material for publication: PLATON (Spek, 2003 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808014359/mg2051sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808014359/mg2051Isup2.hkl

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

[EuBr2(H2O)6]Br	F000 = 456
Mr = 499.79	Dx = 3.006 Mg m−3
Monoclinic, P2/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yc	Cell parameters from 10367 reflections
a = 8.1672 (7) Å	θ = 3.0–32.1º
b = 6.7538 (4) Å	µ = 16.52 mm−1
c = 12.5451 (10) Å	T = 293 (2) K
β = 127.077 (5)º	Irregular polyhedron, clear colourless
V = 552.08 (8) Å3	0.25 × 0.24 × 0.18 mm
Z = 2

Stoe IPDSII diffractometer	1613 independent reflections
Radiation source: fine-focus sealed tube	1397 reflections with I > 2s(I)
Monochromator: graphite	Rint = 0.067
T = 293(2) K	θmax = 30.0º
ω scans (in two runs with φ1 = 0° and φ2 = 90°)	θmin = 3.0º
Absorption correction: numerical[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]	h = −11→11
Tmin = 0.065, Tmax = 0.155	k = −9→9
10921 measured reflections	l = −17→17

Refinement on F2	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F2 > 2σ(F2)] = 0.028	w = 1/[σ2(Fo2) + (0.0169P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.049	(Δ/σ)max < 0.001
S = 1.11	Δρmax = 1.14 e Å−3
1613 reflections	Δρmin = −1.10 e Å−3
72 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0409 (10)
Secondary atom site location: difference Fourier map

Experimental. The title compoud is a commercially available chemical (Alfa Aesar) and was recrystallized under argon from degassed aqueous HBr solution. A suitable single-crystal was sealed with mother liquor in a thin-walled glass capillary.

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
Eu1	0.50000	0.16454 (4)	0.25000	0.0170 (1)
Br1	0.70613 (6)	−0.15845 (7)	0.44669 (4)	0.0295 (1)
Br2	0.00000	0.63151 (9)	0.25000	0.0318 (2)
O1	0.1772 (5)	0.3097 (5)	0.0676 (3)	0.0320 (7)
O2	0.2413 (5)	0.0620 (5)	0.2757 (4)	0.0313 (7)
O3	0.4434 (5)	0.4262 (5)	0.3524 (4)	0.0335 (7)
H11	0.148 (11)	0.336 (10)	−0.006 (4)	0.06 (2)*
H12	0.072 (9)	0.258 (14)	0.050 (10)	0.10 (3)*
H21	0.253 (12)	0.098 (11)	0.342 (5)	0.07 (2)*
H22	0.183 (11)	−0.046 (6)	0.253 (9)	0.09 (3)*
H31	0.518 (10)	0.526 (7)	0.376 (8)	0.08 (2)*
H32	0.321 (5)	0.456 (12)	0.315 (8)	0.09 (3)*

	U11	U22	U33	U12	U13	U23
Eu1	0.0168 (1)	0.0180 (1)	0.0172 (1)	0.000	0.0109 (1)	0.000
Br1	0.0295 (2)	0.0293 (2)	0.0266 (3)	0.0027 (2)	0.0152 (2)	0.0066 (2)
Br2	0.0294 (3)	0.0360 (3)	0.0327 (4)	0.000	0.0202 (3)	0.000
O1	0.0233 (13)	0.0385 (17)	0.0256 (18)	0.0036 (12)	0.0102 (13)	0.0084 (14)
O2	0.0316 (15)	0.0367 (17)	0.0355 (19)	−0.0076 (13)	0.0254 (15)	−0.0055 (14)
O3	0.0308 (15)	0.0302 (15)	0.042 (2)	−0.0035 (13)	0.0229 (16)	−0.0106 (14)

Eu1—Br1	2.9449 (5)	Eu1—O3i	2.388 (3)
Eu1—Br1i	2.9449 (5)	O1—H11	0.82 (2)
Eu1—O1	2.424 (3)	O1—H12	0.83 (2)
Eu1—O1i	2.424 (3)	O2—H21	0.82 (2)
Eu1—O2	2.422 (3)	O2—H22	0.82 (2)
Eu1—O2i	2.422 (3)	O3—H31	0.83 (2)
Eu1—O3	2.388 (3)	O3—H32	0.83 (2)
Br1—Eu1—O1	146.89 (8)	O1—Eu1—O2	72.6 (1)
Br1i—Eu1—O1i	146.89 (8)	O1i—Eu1—O2i	72.6 (1)
Br1—Eu1—O1i	76.21 (9)	O1—Eu1—O2i	122.0 (1)
Br1i—Eu1—O1	76.21 (9)	O1i—Eu1—O2	122.0 (1)
Br1—Eu1—O2	77.33 (8)	O1—Eu1—O3	75.8 (1)
Br1i—Eu1—O2i	77.33 (8)	O1i—Eu1—O3i	75.8 (1)
Br1—Eu1—O2i	78.22 (8)	O1—Eu1—O3i	69.3 (1)
Br1i—Eu1—O2	78.22 (8)	O1i—Eu1—O3	69.3 (1)
Br1—Eu1—O3	107.21 (9)	O2—Eu1—O3	70.9 (1)
Br1i—Eu1—O3i	107.21 (9)	O2i—Eu1—O3i	70.9 (1)
Br1—Eu1—O3i	143.18 (8)	O2—Eu1—O3i	138.6 (1)
Br1i—Eu1—O3	143.18 (8)	O2i—Eu1—O3	138.6 (1)
Br1—Eu1—Br1i	84.41 (2)	H11—O1—H12	104 (8)
O1—Eu1—O1i	132.3 (2)	H21—O2—H22	107 (8)
O2—Eu1—O2i	146.8 (2)	H31—O3—H32	112 (8)
O3—Eu1—O3i	84.5 (2)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···Br2ii	0.83 (2)	2.53 (8)	3.343 (4)	168 (6)
O1—H12···Br1iii	0.83 (2)	2.52 (13)	3.333 (4)	165 (6)
O2—H21···Br1iv	0.82 (2)	2.49 (10)	3.307 (4)	172 (6)
O2—H22···Br2v	0.83 (2)	2.63 (11)	3.417 (4)	161 (6)
O3—H31···Br1vi	0.83 (2)	2.46 (8)	3.288 (4)	173 (6)
O3—H32···Br2	0.83 (2)	2.52 (11)	3.328 (5)	163 (6)

Eu1—Br1	2.9449 (5)
Eu1—O1	2.424 (3)
Eu1—O2	2.422 (3)
Eu1—O3	2.388 (3)

Br1—Eu1—O1	146.89 (8)
Br1—Eu1—O1i	76.21 (9)
Br1—Eu1—O2	77.33 (8)
Br1—Eu1—O2i	78.22 (8)
Br1—Eu1—O3	107.21 (9)
Br1—Eu1—O3i	143.18 (8)
Br1—Eu1—Br1i	84.41 (2)
O1—Eu1—O1i	132.3 (2)
O2—Eu1—O2i	146.8 (2)
O3—Eu1—O3i	84.5 (2)
O1—Eu1—O2	72.6 (1)
O1—Eu1—O2i	122.0 (1)
O1—Eu1—O3	75.8 (1)
O1—Eu1—O3i	69.3 (1)
O2—Eu1—O3	70.9 (1)
O2—Eu1—O3i	138.6 (1)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H11⋯Br2ii	0.83 (2)	2.53 (8)	3.343 (4)	168 (6)
O1—H12⋯Br1iii	0.83 (2)	2.52 (13)	3.333 (4)	165 (6)
O2—H21⋯Br1iv	0.82 (2)	2.49 (10)	3.307 (4)	172 (6)
O2—H22⋯Br2v	0.83 (2)	2.63 (11)	3.417 (4)	161 (6)
O3—H31⋯Br1vi	0.83 (2)	2.46 (8)	3.288 (4)	173 (6)
O3—H32⋯Br2	0.83 (2)	2.52 (11)	3.328 (5)	163 (6)

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) ; (vi) .