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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807055006/si2044sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807055006/si2044Isup2.hkl
Contains datablock I

CCDC reference: 672604

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.021
  • wR factor = 0.047
  • Data-to-parameter ratio = 16.3

checkCIF/PLATON results

No syntax errors found



Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Sm (3) 3.25
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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

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]F(000) = 1408
Mr = 745.00Dx = 2.346 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 258 reflections
a = 13.9896 (2) Åθ = 3.3–26.7°
b = 6.8923 (1) ŵ = 5.58 mm1
c = 21.8748 (3) ÅT = 291 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)
Graphite monochromatorRint = 0.034
ϕ and ω scansθmax = 28.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1618
Tmin = 0.215, Tmax = 0.455k = 89
11742 measured reflectionsl = 2528
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021H-atom parameters constrained
wR(F2) = 0.047 w = 1/[σ2(Fo2) + (0.010P)2 + 2.1343P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.010
2521 reflectionsΔρmax = 0.66 e Å3
155 parametersΔρmin = 0.65 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00015 (4)
Crystal data top
[Sm2(C4H4O4)(C8H4O4)2]V = 2109.18 (5) Å3
Mr = 745.00Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 13.9896 (2) ŵ = 5.58 mm1
b = 6.8923 (1) ÅT = 291 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)] = 0.0210 restraints
wR(F2) = 0.047H-atom parameters constrained
S = 1.03Δρmax = 0.66 e Å3
2521 reflectionsΔρmin = 0.65 e Å3
155 parameters
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, º) 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, z1/2; (iii) x, y+3/2, z1/2; (iv) x+3/2, y1/2, 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.

Experimental details

Crystal data
Chemical formula[Sm2(C4H4O4)(C8H4O4)2]
Mr745.00
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)291
a, b, c (Å)13.9896 (2), 6.8923 (1), 21.8748 (3)
V3)2109.18 (5)
Z4
Radiation typeMo Kα
µ (mm1)5.58
Crystal size (mm)0.30 × 0.24 × 0.14
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.215, 0.455
No. of measured, independent and
observed [I > 2σ(I)] reflections
11742, 2521, 2028
Rint0.034
(sin θ/λ)max1)0.661
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.021, 0.047, 1.03
No. of reflections2521
No. of parameters155
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.66, 0.65

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998).

Selected bond lengths (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, z1/2; (iii) x, y+3/2, z1/2; (iv) x+3/2, y1/2, z; (v) x+3/2, y+1/2, z.
 

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