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Acta Cryst. (2007). E63, m2922    [ doi:10.1107/S1600536807054414 ]

Poly[di-[mu]4-benzene-1,4-dicarboxylato-[mu]6-succinato-dieuropium(III)]

Q. He and B.-J. Huang

Abstract top

The title compound, [Eu2(C4H4O4)(C8H4O4)2]n, has been synthesized by hydrothermal methods. The Eu atom is coordinated by four O atoms from four benzene-1,4-dicarboxylate (BDC) anions and four O atoms from three succinate anions in a distorted square antiprismatic coordination geometry. The antiprisms are bridged by the benzene-1,4-dicarboxylate and succinate anions into a three-dimensional coordination network. The succinate anions are located on centres of inversion.

Comment top

The title compound, (I), is isostructural with its [M2(C8H4O4)2(C4H4O4)]n [M = Gd (Wang & Li, 2005), Dy ((Li & Wang, 2005), Nd (Li et al., 2006) and Er (He et al., 2006)] analogues. The Eu3+ ion is located at the center of a distorted square antiprism and is coordinated by four oxygen atoms from four benzene-1,4-dicarboxylate anions and four oxygen atoms from three succinate anions (Fig. 1). The Eu—O bond distances ranging from 2.2851 (2) to 2.5764 (16) Å.

The succinate anions are located on centres of inversion and acts as a bis-chelating ligands for each two symmetry related Eu atoms. Each of the four oxygen atom are additionally connected by Eu atoms into layers which are parallel to the (001) plane. These layers are connected via the benzene-1,4-dicarboxylate anions into a three-dimensional coordination network.

Related literature top

For related literature, see: Li & Wang (2005), Li et al. (2006), Wang & Li (2005) and He et al. (2006).

Experimental top

A mixture of EuCl3·6H2O (2.00 mmol, 0.73 g), benzene-1,4-dicarboxylic acid (1.0 mmol, 0.16 g), succinic acid (1.0 mmol, 0.10 g), NaOH (6.0 ml, 1 mol/L) and H2O (20.0 ml) was heated in a 35 ml stainless steel autoclave with a teflon liner at 453 K for 48 h. After cooling to room temperature column-like crystals of the title compound has formed which were filtered off and washed with ethanol. Yield: 7% based on Eu.

Refinement top

The H atoms were included at calculated positions and treated as riding atoms, with C—H distances of 0.93–0.97 Å and Uiso(H) = 1.2Ueq(C)].

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).

Figures top
[Figure 1] Fig. 1. The coordination environment of the Eu atom, with the atom-numbering scheme and displacement ellipsoids drawn at the 50% probability level. Symmetry codes: (i) 2 − x, 2 − y, 1 − z; (ii) 3/2 − x, 2 − y, z − 1/2; (iii) x, 3/2 − y, z − 1/2; (iv) 3/2 − x, y + 1/2, z; (v) 3/2 − x, y − 1/2, z; (vi) 1 − x, 2 − y, 1 − z.
Poly[di-µ4-benzene-1,4-dicarboxylato-µ6-succinato-dieuropium(III)] top
Crystal data top
[Eu2(C4H4O4)(C8H4O4)2]F000 = 1416
Mr = 374.11Dx = 2.374 Mg m−3
Orthorhombic, PbcaMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 124 reflections
a = 13.9501 (3) Åθ = 3.3–26.7º
b = 6.86960 (10) ŵ = 6.01 mm−1
c = 21.8409 (4) ÅT = 292 (2) K
V = 2093.05 (7) Å3Column, orange
Z = 80.26 × 0.21 × 0.15 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		2458 independent reflections
Radiation source: fine-focus sealed tube2083 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.020
T = 292(2) Kθmax = 28.0º
φ and ω scansθmin = 1.9º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −18→15
Tmin = 0.232, Tmax = 0.415k = −7→9
11756 measured reflectionsl = −28→28
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.016  w = 1/[σ2(Fo2) + (0.0182P)2 + 0.8889P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.040(Δ/σ)max = 0.014
S = 1.10Δρmax = 0.73 e Å−3
2458 reflectionsΔρmin = −0.46 e Å−3
155 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00043 (4)
Secondary atom site location: difference Fourier map
Crystal data top
[Eu2(C4H4O4)(C8H4O4)2]V = 2093.05 (7) Å3
Mr = 374.11Z = 8
Orthorhombic, PbcaMo Kα
a = 13.9501 (3) ŵ = 6.01 mm−1
b = 6.86960 (10) ÅT = 292 (2) K
c = 21.8409 (4) Å0.26 × 0.21 × 0.15 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		2458 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		2083 reflections with I > 2σ(I)
Tmin = 0.232, Tmax = 0.415Rint = 0.020
11756 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.016155 parameters
wR(F2) = 0.040H-atom parameters constrained
S = 1.10Δρmax = 0.73 e Å−3
2458 reflectionsΔρmin = −0.46 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
xyzUiso*/Ueq
Eu0.831538 (8)1.019333 (16)0.445256 (5)0.01307 (5)
O10.86262 (14)1.0402 (3)0.55012 (7)0.0207 (4)
O21.00832 (12)0.9242 (3)0.56773 (7)0.0218 (4)
C10.92483 (18)0.9674 (3)0.58479 (10)0.0156 (5)
C20.89791 (18)0.9259 (3)0.65008 (10)0.0175 (5)
C30.8072 (2)0.9723 (4)0.67128 (12)0.0257 (6)
H3A0.76291.02960.64500.031*
C40.7821 (2)0.9335 (4)0.73152 (11)0.0278 (6)
H4A0.72100.96450.74550.033*
C50.84800 (18)0.8486 (4)0.77108 (11)0.0216 (5)
C60.82002 (19)0.7999 (4)0.83558 (11)0.0231 (6)
C70.9384 (2)0.8024 (4)0.74985 (11)0.0291 (6)
H7A0.98280.74570.77620.035*
C80.96347 (19)0.8400 (4)0.68955 (11)0.0280 (6)
H8A1.02440.80760.67550.034*
O30.74136 (14)0.8621 (3)0.85578 (8)0.0294 (4)
O40.87738 (14)0.6966 (3)0.86622 (8)0.0312 (4)
O50.66579 (12)0.8740 (3)0.45395 (8)0.0238 (4)
O60.67471 (12)1.1767 (2)0.48308 (8)0.0202 (4)
C90.6250 (2)1.0308 (4)0.46890 (13)0.0231 (6)
C100.5164 (2)1.0421 (4)0.46964 (14)0.0297 (6)
H10A0.48970.96780.43590.036*
H10B0.49551.17620.46580.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Eu0.01286 (8)0.01546 (8)0.01090 (7)−0.00057 (4)0.00000 (4)−0.00124 (4)
O10.0211 (10)0.0280 (10)0.0130 (9)0.0020 (7)−0.0006 (7)0.0010 (7)
O20.0158 (10)0.0323 (10)0.0173 (9)−0.0014 (8)0.0043 (7)0.0021 (7)
C10.0182 (13)0.0162 (12)0.0124 (12)−0.0030 (9)0.0015 (10)−0.0021 (9)
C20.0196 (14)0.0214 (12)0.0117 (11)0.0003 (10)0.0022 (10)0.0024 (9)
C30.0244 (15)0.0341 (15)0.0185 (14)0.0086 (11)0.0028 (11)0.0071 (11)
C40.0251 (16)0.0375 (16)0.0209 (14)0.0081 (12)0.0121 (12)0.0045 (12)
C50.0276 (16)0.0229 (13)0.0142 (12)0.0001 (10)0.0062 (11)0.0017 (10)
C60.0351 (17)0.0198 (13)0.0143 (12)−0.0047 (11)0.0056 (11)0.0016 (10)
C70.0276 (17)0.0413 (17)0.0184 (13)0.0056 (12)0.0006 (12)0.0100 (11)
C80.0221 (15)0.0420 (17)0.0200 (14)0.0070 (12)0.0062 (12)0.0070 (11)
O30.0317 (12)0.0397 (12)0.0170 (9)0.0004 (9)0.0092 (8)−0.0031 (8)
O40.0408 (12)0.0309 (11)0.0219 (10)0.0037 (9)0.0076 (9)0.0101 (8)
O50.0181 (10)0.0145 (9)0.0388 (11)0.0010 (7)0.0061 (8)−0.0017 (7)
O60.0201 (10)0.0166 (9)0.0241 (9)−0.0026 (7)0.0017 (7)−0.0017 (7)
C90.0180 (14)0.0218 (14)0.0295 (14)−0.0010 (10)0.0096 (12)0.0012 (11)
C100.0326 (18)0.0235 (14)0.0331 (16)0.0028 (12)0.0012 (13)0.0018 (12)
Geometric parameters (Å, °) top
Eu—O12.3355 (16)C4—C51.390 (3)
Eu—O2i2.2851 (17)C4—H4A0.9300
Eu—O3ii2.3486 (17)C5—C71.381 (3)
Eu—O4iii2.3642 (17)C5—C61.499 (3)
Eu—O5iv2.4440 (18)C6—O31.258 (3)
Eu—O52.5257 (17)C6—O41.261 (3)
Eu—O6v2.4958 (17)C7—C81.387 (3)
Eu—O62.5764 (16)C7—H7A0.9300
Eu—Euv4.11984 (14)C8—H8A0.9300
O1—C11.256 (3)O5—C91.262 (3)
O2—C11.258 (3)O6—C91.258 (3)
C1—C21.502 (3)C9—C101.517 (4)
C2—C31.385 (4)C10—C10vi1.517 (6)
C2—C81.388 (3)C10—H10A0.9700
C3—C41.387 (4)C10—H10B0.9700
C3—H3A0.9300
O2i—Eu—O185.98 (6)C4—C5—C6120.4 (2)
O2i—Eu—O3ii105.14 (6)O3—C6—O4124.0 (2)
O1—Eu—O3ii151.06 (6)O3—C6—C5118.7 (2)
O2i—Eu—O4iii75.60 (6)O4—C6—C5117.3 (2)
O1—Eu—O4iii134.78 (6)C5—C6—Euvii146.06 (16)
O3ii—Eu—O4iii74.16 (7)C5—C7—C8120.4 (2)
O2i—Eu—O5iv79.96 (6)C5—C7—H7A119.8
O1—Eu—O5iv81.94 (6)C8—C7—H7A119.8
O4iii—Eu—O5iv132.70 (6)C7—C8—C2120.2 (2)
O2i—Eu—O6v103.61 (6)C7—C8—H8A119.9
O3ii—Eu—O6v125.96 (6)C2—C8—H8A119.9
O4iii—Eu—O6v70.09 (6)C6—O3—Euviii141.96 (17)
O3ii—Eu—O578.65 (6)C6—O4—Euvii124.66 (17)
O5iv—Eu—O5113.72 (5)C9—O5—Euv151.43 (17)
O1—Eu—O679.48 (6)C9—O5—Eu95.47 (15)
O5iv—Eu—O664.51 (5)Euv—O5—Eu111.98 (6)
O6v—Eu—O6105.07 (5)C9—O6—Euiv130.59 (17)
O1—C1—O2123.7 (2)C9—O6—Eu93.16 (15)
O1—C1—C2118.4 (2)Euiv—O6—Eu108.62 (6)
O2—C1—C2117.9 (2)O6—C9—O5119.7 (2)
C3—C2—C8119.5 (2)O6—C9—C10120.5 (2)
C3—C2—C1120.1 (2)O5—C9—C10119.8 (2)
C8—C2—C1120.4 (2)O6—C9—Eu61.44 (13)
C2—C3—C4120.2 (2)O5—C9—Eu59.14 (13)
C2—C3—H3A119.9C10—C9—Eu170.36 (19)
C4—C3—H3A119.9C9—C10—C10vi106.9 (3)
C3—C4—C5120.3 (2)C9—C10—H10A110.3
C3—C4—H4A119.9C10vi—C10—H10A110.3
C5—C4—H4A119.9C9—C10—H10B110.3
C7—C5—C4119.5 (2)C10vi—C10—H10B110.3
C7—C5—C6120.1 (2)H10A—C10—H10B108.6
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) −x+3/2, −y+2, z−1/2; (iii) x, −y+3/2, z−1/2; (iv) −x+3/2, y+1/2, z; (v) −x+3/2, y−1/2, z; (vi) −x+1, −y+2, −z+1; (vii) x, −y+3/2, z+1/2; (viii) −x+3/2, −y+2, z+1/2.
Table 1
Selected geometric parameters (Å) top
Eu—O12.3355 (16)Eu—O5iv2.4440 (18)
Eu—O2i2.2851 (17)Eu—O52.5257 (17)
Eu—O3ii2.3486 (17)Eu—O6v2.4958 (17)
Eu—O4iii2.3642 (17)Eu—O62.5764 (16)
Symmetry codes: (i) −x+2, −y+2, −z+1; (ii) −x+3/2, −y+2, z−1/2; (iii) x, −y+3/2, z−1/2; (iv) −x+3/2, y+1/2, z; (v) −x+3/2, y−1/2, z.
Acknowledgements top

Any acknowledgements?

references
References top

Bruker (1998). SMART (Version 5.16), SAINT (Version 6.01) and SHELXTL (Version 6.14). Bruker AXS Inc., Madison, Wisconsin, USA.

He, Q., Zi, J.-F. & Zhang, F.-J. (2006). Acta Cryst. E62, m997–m998.

Li, Z.-F. & Wang, C.-X. (2005). Acta Cryst. E61, m2689–m2690.

Li, Z.-F., Wang, C.-X., Li, Y., Cai, D.-J. & Xiao, Y.-J. (2006). Acta Cryst. E62, m251–m252.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Wang, C.-X. & Li, Z.-F. (2005). Acta Cryst. E61, m2212–m2213.