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Acta Cryst. (2007). E63, m2923    [ doi:10.1107/S1600536807055006 ]

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

Q. He and B.-J. Huang

Abstract top

The title compound, [Sm2(C4H4O4)(C8H4O4)2]n, has been hydrothermally synthesized. The Sm atom is coordinated by four O atoms from four benzene-1,4-dicarboxylate (BDC) ligands and four O atoms from three succinate anions in a distorted square antiprismatic geometry. The antiprisms are bridged by the BDC and succinate ligands, forming a three-dimensional network. The succinate ion is located on a centre 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), Er (He et al., 2006)] analogues. As depicted in Fig.1, The Sm3+ ion is located at the center of a distorted square antiprism geometry and is coordinated by four O atoms from four BDC and four O atoms from three succinate anions. The Sm—O bond distances range from 2.298 (2) to 2.591 (2) Å.

In (I), the succinate ligand is located on an inversion centre and functions as an octadentate ligand, bis-chelating two Sm atoms with each O atom bridging to another Sm atom. In this mode, the Sm atoms are linked into a two-dimensional polymeric sheet parallel to the (001) plane. These sheets are in turn bridged via BDC ligands, forming a three-dimensional framework.

Related literature top

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

Experimental top

A mixture of SmCl3·6H2O (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 reactor with a Teflon liner at 453 K for 48 h. The column-like crystals were filtered and washed with ethanol. Yield: 5% based on Sm.

Refinement top

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 Sm atom, with the atom-numbering scheme, showing 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-disamarium(III)] top
Crystal data top
[Sm2(C4H4O4)(C8H4O4)2]F000 = 1408
Mr = 745.00Dx = 2.346 Mg m−3
Orthorhombic, PbcaMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 258 reflections
a = 13.9896 (2) Åθ = 3.3–26.7º
b = 6.8923 (1) ŵ = 5.58 mm−1
c = 21.8748 (3) ÅT = 291 (2) K
V = 2109.18 (5) Å3Column, colorless
Z = 40.30 × 0.24 × 0.14 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		2521 independent reflections
Radiation source: fine-focus sealed tube2028 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.034
T = 291(2) Kθmax = 28.0º
φ and ω scansθmin = 1.9º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −16→18
Tmin = 0.215, Tmax = 0.455k = −8→9
11742 measured reflectionsl = −25→28
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.021  w = 1/[σ2(Fo2) + (0.010P)2 + 2.1343P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.047(Δ/σ)max = 0.010
S = 1.03Δρmax = 0.66 e Å−3
2521 reflectionsΔρmin = −0.65 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: 0.00015 (4)
Secondary atom site location: difference Fourier map
Crystal data top
[Sm2(C4H4O4)(C8H4O4)2]V = 2109.18 (5) Å3
Mr = 745.00Z = 4
Orthorhombic, PbcaMo Kα
a = 13.9896 (2) ŵ = 5.58 mm−1
b = 6.8923 (1) ÅT = 291 (2) K
c = 21.8748 (3) Å0.30 × 0.24 × 0.14 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		2521 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		2028 reflections with I > 2σ(I)
Tmin = 0.215, Tmax = 0.455Rint = 0.034
11742 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.021155 parameters
wR(F2) = 0.047H-atom parameters constrained
S = 1.03Δρmax = 0.66 e Å−3
2521 reflectionsΔρmin = −0.65 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
Sm0.831769 (9)1.01978 (2)0.445280 (7)0.01351 (6)
O10.86274 (16)1.0413 (3)0.55071 (9)0.0213 (5)
O21.00773 (15)0.9231 (3)0.56802 (10)0.0226 (5)
C10.9245 (2)0.9670 (4)0.58552 (13)0.0162 (6)
C20.8979 (2)0.9258 (5)0.65030 (13)0.0179 (6)
C30.8072 (2)0.9726 (5)0.67140 (16)0.0275 (8)
H3A0.76291.02970.64520.033*
C40.7827 (2)0.9339 (5)0.73188 (15)0.0283 (8)
H4A0.72200.96580.74600.034*
C50.8480 (2)0.8480 (5)0.77128 (15)0.0234 (7)
C60.8204 (2)0.7994 (5)0.83569 (15)0.0244 (7)
C70.9386 (2)0.8012 (6)0.74961 (16)0.0310 (8)
H7A0.98280.74410.77570.037*
C80.9635 (2)0.8391 (5)0.68950 (15)0.0276 (8)
H8A1.02410.80650.67540.033*
O30.74192 (17)0.8604 (4)0.85596 (10)0.0314 (6)
O40.87809 (19)0.6959 (4)0.86582 (11)0.0336 (6)
O50.67416 (15)1.1773 (3)0.48285 (10)0.0213 (5)
O60.66547 (15)0.8740 (3)0.45425 (11)0.0247 (5)
C90.6247 (2)1.0309 (5)0.46912 (17)0.0234 (7)
C100.5163 (2)1.0420 (5)0.46982 (17)0.0292 (8)
H10A0.49541.17570.46610.035*
H10B0.48970.96820.43610.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sm0.01370 (9)0.01523 (10)0.01160 (9)−0.00074 (5)−0.00012 (5)−0.00132 (6)
O10.0238 (11)0.0261 (13)0.0141 (12)0.0017 (9)−0.0008 (8)0.0010 (10)
O20.0178 (11)0.0329 (13)0.0171 (11)−0.0004 (10)0.0051 (9)0.0015 (10)
C10.0209 (15)0.0168 (16)0.0109 (15)−0.0034 (11)0.0016 (11)0.0003 (12)
C20.0233 (15)0.0170 (17)0.0133 (15)−0.0002 (12)0.0024 (12)0.0035 (12)
C30.0269 (16)0.034 (2)0.0213 (18)0.0129 (14)0.0048 (13)0.0048 (15)
C40.0275 (18)0.037 (2)0.0208 (17)0.0083 (15)0.0108 (14)0.0023 (16)
C50.0367 (19)0.0186 (17)0.0151 (16)0.0012 (13)0.0066 (14)0.0037 (13)
C60.0316 (18)0.0246 (18)0.0170 (16)−0.0059 (14)0.0046 (14)−0.0003 (14)
C70.0291 (18)0.042 (2)0.0214 (18)0.0072 (15)0.0010 (14)0.0135 (17)
C80.0222 (16)0.040 (2)0.0202 (18)0.0047 (14)0.0049 (13)0.0100 (16)
O30.0328 (14)0.0406 (16)0.0208 (12)−0.0007 (11)0.0086 (10)−0.0023 (11)
O40.0457 (15)0.0327 (15)0.0226 (13)0.0043 (12)0.0087 (11)0.0107 (11)
O50.0219 (12)0.0163 (12)0.0257 (13)−0.0014 (9)0.0024 (9)−0.0031 (9)
O60.0191 (11)0.0155 (12)0.0397 (15)0.0029 (9)0.0081 (10)−0.0011 (10)
C90.0202 (16)0.0201 (19)0.0299 (19)−0.0007 (13)0.0100 (13)0.0004 (15)
C100.0306 (19)0.023 (2)0.034 (2)0.0050 (14)0.0060 (15)0.0029 (16)
Geometric parameters (Å, °) top
Sm—O12.351 (2)C4—C51.388 (5)
Sm—O2i2.298 (2)C4—H4A0.9300
Sm—O3ii2.359 (2)C5—C71.391 (5)
Sm—O4iii2.377 (2)C5—C61.499 (4)
Sm—O5iv2.501 (2)C6—O31.257 (4)
Sm—O52.591 (2)C6—O41.262 (4)
Sm—O6v2.450 (2)C7—C81.385 (4)
Sm—O62.542 (2)C7—H7A0.9300
O1—C11.260 (4)C8—H8A0.9300
O2—C11.263 (4)O5—C91.260 (4)
C1—C21.492 (4)O6—C91.265 (4)
C2—C31.389 (4)C9—C101.519 (5)
C2—C81.391 (4)C10—C10vi1.512 (7)
C3—C41.392 (5)C10—H10A0.9700
C3—H3A0.9300C10—H10B0.9700
O2i—Sm—O186.17 (8)C3—C2—C8119.9 (3)
O2i—Sm—O3ii105.20 (8)C3—C2—C1119.9 (3)
O1—Sm—O3ii150.58 (8)C8—C2—C1120.2 (3)
O2i—Sm—O4iii75.42 (8)C2—C3—C4119.7 (3)
O1—Sm—O4iii134.93 (9)C2—C3—H3A120.1
O3ii—Sm—O4iii74.49 (9)C4—C3—H3A120.1
O2i—Sm—O6v79.86 (8)C5—C4—C3120.7 (3)
O1—Sm—O6v81.71 (8)C5—C4—H4A119.7
O3ii—Sm—O6v73.99 (8)C3—C4—H4A119.7
O4iii—Sm—O6v132.66 (8)C4—C5—C7119.1 (3)
O2i—Sm—O5iv103.63 (8)C4—C5—C6120.7 (3)
O1—Sm—O5iv75.12 (7)C7—C5—C6120.2 (3)
O3ii—Sm—O5iv126.04 (8)O3—C6—O4124.3 (3)
O4iii—Sm—O5iv70.06 (8)O3—C6—C5118.8 (3)
O6v—Sm—O5iv156.20 (8)O4—C6—C5116.9 (3)
O2i—Sm—O6166.37 (7)C8—C7—C5120.6 (3)
O1—Sm—O696.77 (8)C8—C7—H7A119.7
O3ii—Sm—O678.60 (8)C5—C7—H7A119.7
O4iii—Sm—O693.37 (8)C7—C8—C2120.0 (3)
O6v—Sm—O6113.71 (6)C7—C8—H8A120.0
O5iv—Sm—O664.61 (7)C2—C8—H8A120.0
O2i—Sm—O5143.10 (7)C6—O3—Smvii142.3 (2)
O1—Sm—O579.60 (7)C6—O4—Smviii124.1 (2)
O3ii—Sm—O575.17 (8)C9—O5—Smv131.3 (2)
O4iii—Sm—O5136.53 (8)C9—O5—Sm93.21 (18)
O6v—Sm—O564.56 (7)Smv—O5—Sm108.63 (8)
O5iv—Sm—O5105.25 (6)C9—O6—Smiv151.6 (2)
O6—Sm—O550.38 (7)C9—O6—Sm95.45 (18)
O2i—Sm—C9168.31 (9)Smiv—O6—Sm111.92 (8)
O1—Sm—C990.34 (9)O5—C9—O6119.9 (3)
O3ii—Sm—C973.00 (9)O5—C9—C10120.4 (3)
O4iii—Sm—C9114.45 (9)O6—C9—C10119.8 (3)
O6v—Sm—C988.60 (8)O5—C9—Sm61.49 (16)
O5iv—Sm—C986.19 (8)O6—C9—Sm59.24 (15)
O6—Sm—C925.31 (8)C10—C9—Sm170.3 (3)
O5—Sm—C925.30 (8)C10vi—C10—C9106.8 (4)
C1—O1—Sm133.9 (2)C10vi—C10—H10A110.4
C1—O2—Smi154.0 (2)C9—C10—H10A110.4
O1—C1—O2123.1 (3)C10vi—C10—H10B110.4
O1—C1—C2118.7 (3)C9—C10—H10B110.4
O2—C1—C2118.2 (3)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+3/2, −y+2, z+1/2; (viii) x, −y+3/2, z+1/2.
Table 1
Selected geometric parameters (Å) top
Sm—O12.351 (2)Sm—O5iv2.501 (2)
Sm—O2i2.298 (2)Sm—O52.591 (2)
Sm—O3ii2.359 (2)Sm—O6v2.450 (2)
Sm—O4iii2.377 (2)Sm—O62.542 (2)
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.
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.