Poly[di-μ₄-benzene-1,4-dicarboxyl­ato-μ₆-succinato-dieuropium(III)]

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.

Key indicators

• Single-crystal X-ray study
• T = 292 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.016
• wR factor = 0.040
• Data-to-parameter ratio = 15.9

checkCIF/PLATON results

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Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for Eu          (3)       3.23

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   0 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
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S1. Comment

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

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

S2. Experimental

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.

S3. Refinement

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

Computing details

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

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)]

Crystal data

[Eu2(C4H4O4)(C8H4O4)2]	F(000) = 1416
Mr = 374.11	Dx = 2.374 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 124 reflections
a = 13.9501 (3) Å	θ = 3.3–26.7°
b = 6.8696 (1) Å	µ = 6.01 mm^−1
c = 21.8409 (4) Å	T = 292 K
V = 2093.05 (7) Å^3	Column, orange
Z = 8	0.26 × 0.21 × 0.15 mm

Data collection

Bruker SMART CCD area-detector diffractometer	2458 independent reflections
Radiation source: fine-focus sealed tube	2083 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
ϕ and ω scans	θmax = 28.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −18→15
Tmin = 0.232, Tmax = 0.415	k = −7→9
11756 measured reflections	l = −28→28

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.016	H-atom parameters constrained
wR(F^2) = 0.040	w = 1/[σ^2(Fo^2) + (0.0182P)^2 + 0.8889P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max = 0.014
2458 reflections	Δρmax = 0.73 e Å^−3
155 parameters	Δρmin = −0.46 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00043 (4)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Eu	0.831538 (8)	1.019333 (16)	0.445256 (5)	0.01307 (5)
O1	0.86262 (14)	1.0402 (3)	0.55012 (7)	0.0207 (4)
O2	1.00832 (12)	0.9242 (3)	0.56773 (7)	0.0218 (4)
C1	0.92483 (18)	0.9674 (3)	0.58479 (10)	0.0156 (5)
C2	0.89791 (18)	0.9259 (3)	0.65008 (10)	0.0175 (5)
C3	0.8072 (2)	0.9723 (4)	0.67128 (12)	0.0257 (6)
H3A	0.7629	1.0296	0.6450	0.031*
C4	0.7821 (2)	0.9335 (4)	0.73152 (11)	0.0278 (6)
H4A	0.7210	0.9645	0.7455	0.033*
C5	0.84800 (18)	0.8486 (4)	0.77108 (11)	0.0216 (5)
C6	0.82002 (19)	0.7999 (4)	0.83558 (11)	0.0231 (6)
C7	0.9384 (2)	0.8024 (4)	0.74985 (11)	0.0291 (6)
H7A	0.9828	0.7457	0.7762	0.035*
C8	0.96347 (19)	0.8400 (4)	0.68955 (11)	0.0280 (6)
H8A	1.0244	0.8076	0.6755	0.034*
O3	0.74136 (14)	0.8621 (3)	0.85578 (8)	0.0294 (4)
O4	0.87738 (14)	0.6966 (3)	0.86622 (8)	0.0312 (4)
O5	0.66579 (12)	0.8740 (3)	0.45395 (8)	0.0238 (4)
O6	0.67471 (12)	1.1767 (2)	0.48308 (8)	0.0202 (4)
C9	0.6250 (2)	1.0308 (4)	0.46890 (13)	0.0231 (6)
C10	0.5164 (2)	1.0421 (4)	0.46964 (14)	0.0297 (6)
H10A	0.4897	0.9678	0.4359	0.036*
H10B	0.4955	1.1762	0.4658	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Eu	0.01286 (8)	0.01546 (8)	0.01090 (7)	−0.00057 (4)	0.00000 (4)	−0.00124 (4)
O1	0.0211 (10)	0.0280 (10)	0.0130 (9)	0.0020 (7)	−0.0006 (7)	0.0010 (7)
O2	0.0158 (10)	0.0323 (10)	0.0173 (9)	−0.0014 (8)	0.0043 (7)	0.0021 (7)
C1	0.0182 (13)	0.0162 (12)	0.0124 (12)	−0.0030 (9)	0.0015 (10)	−0.0021 (9)
C2	0.0196 (14)	0.0214 (12)	0.0117 (11)	0.0003 (10)	0.0022 (10)	0.0024 (9)
C3	0.0244 (15)	0.0341 (15)	0.0185 (14)	0.0086 (11)	0.0028 (11)	0.0071 (11)
C4	0.0251 (16)	0.0375 (16)	0.0209 (14)	0.0081 (12)	0.0121 (12)	0.0045 (12)
C5	0.0276 (16)	0.0229 (13)	0.0142 (12)	0.0001 (10)	0.0062 (11)	0.0017 (10)
C6	0.0351 (17)	0.0198 (13)	0.0143 (12)	−0.0047 (11)	0.0056 (11)	0.0016 (10)
C7	0.0276 (17)	0.0413 (17)	0.0184 (13)	0.0056 (12)	0.0006 (12)	0.0100 (11)
C8	0.0221 (15)	0.0420 (17)	0.0200 (14)	0.0070 (12)	0.0062 (12)	0.0070 (11)
O3	0.0317 (12)	0.0397 (12)	0.0170 (9)	0.0004 (9)	0.0092 (8)	−0.0031 (8)
O4	0.0408 (12)	0.0309 (11)	0.0219 (10)	0.0037 (9)	0.0076 (9)	0.0101 (8)
O5	0.0181 (10)	0.0145 (9)	0.0388 (11)	0.0010 (7)	0.0061 (8)	−0.0017 (7)
O6	0.0201 (10)	0.0166 (9)	0.0241 (9)	−0.0026 (7)	0.0017 (7)	−0.0017 (7)
C9	0.0180 (14)	0.0218 (14)	0.0295 (14)	−0.0010 (10)	0.0096 (12)	0.0012 (11)
C10	0.0326 (18)	0.0235 (14)	0.0331 (16)	0.0028 (12)	0.0012 (13)	0.0018 (12)

Geometric parameters (Å, º)

Eu—O1	2.3355 (16)	C4—C5	1.390 (3)
Eu—O2^i	2.2851 (17)	C4—H4A	0.9300
Eu—O3^ii	2.3486 (17)	C5—C7	1.381 (3)
Eu—O4^iii	2.3642 (17)	C5—C6	1.499 (3)
Eu—O5^iv	2.4440 (18)	C6—O3	1.258 (3)
Eu—O5	2.5257 (17)	C6—O4	1.261 (3)
Eu—O6^v	2.4958 (17)	C7—C8	1.387 (3)
Eu—O6	2.5764 (16)	C7—H7A	0.9300
Eu—Eu^v	4.1198 (1)	C8—H8A	0.9300
O1—C1	1.256 (3)	O5—C9	1.262 (3)
O2—C1	1.258 (3)	O6—C9	1.258 (3)
C1—C2	1.502 (3)	C9—C10	1.517 (4)
C2—C3	1.385 (4)	C10—C10^vi	1.517 (6)
C2—C8	1.388 (3)	C10—H10A	0.9700
C3—C4	1.387 (4)	C10—H10B	0.9700
C3—H3A	0.9300
O2^i—Eu—O1	85.98 (6)	C4—C5—C6	120.4 (2)
O2^i—Eu—O3^ii	105.14 (6)	O3—C6—O4	124.0 (2)
O1—Eu—O3^ii	151.06 (6)	O3—C6—C5	118.7 (2)
O2^i—Eu—O4^iii	75.60 (6)	O4—C6—C5	117.3 (2)
O1—Eu—O4^iii	134.78 (6)	C5—C6—Eu^vii	146.06 (16)
O3^ii—Eu—O4^iii	74.16 (7)	C5—C7—C8	120.4 (2)
O2^i—Eu—O5^iv	79.96 (6)	C5—C7—H7A	119.8
O1—Eu—O5^iv	81.94 (6)	C8—C7—H7A	119.8
O4^iii—Eu—O5^iv	132.70 (6)	C7—C8—C2	120.2 (2)
O2^i—Eu—O6^v	103.61 (6)	C7—C8—H8A	119.9
O3^ii—Eu—O6^v	125.96 (6)	C2—C8—H8A	119.9
O4^iii—Eu—O6^v	70.09 (6)	C6—O3—Eu^viii	141.96 (17)
O3^ii—Eu—O5	78.65 (6)	C6—O4—Eu^vii	124.66 (17)
O5^iv—Eu—O5	113.72 (5)	C9—O5—Eu^v	151.43 (17)
O1—Eu—O6	79.48 (6)	C9—O5—Eu	95.47 (15)
O5^iv—Eu—O6	64.51 (5)	Eu^v—O5—Eu	111.98 (6)
O6^v—Eu—O6	105.07 (5)	C9—O6—Eu^iv	130.59 (17)
O1—C1—O2	123.7 (2)	C9—O6—Eu	93.16 (15)
O1—C1—C2	118.4 (2)	Eu^iv—O6—Eu	108.62 (6)
O2—C1—C2	117.9 (2)	O6—C9—O5	119.7 (2)
C3—C2—C8	119.5 (2)	O6—C9—C10	120.5 (2)
C3—C2—C1	120.1 (2)	O5—C9—C10	119.8 (2)
C8—C2—C1	120.4 (2)	O6—C9—Eu	61.44 (13)
C2—C3—C4	120.2 (2)	O5—C9—Eu	59.14 (13)
C2—C3—H3A	119.9	C10—C9—Eu	170.36 (19)
C4—C3—H3A	119.9	C9—C10—C10^vi	106.9 (3)
C3—C4—C5	120.3 (2)	C9—C10—H10A	110.3
C3—C4—H4A	119.9	C10^vi—C10—H10A	110.3
C5—C4—H4A	119.9	C9—C10—H10B	110.3
C7—C5—C4	119.5 (2)	C10^vi—C10—H10B	110.3
C7—C5—C6	120.1 (2)	H10A—C10—H10B	108.6

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.