Poly[[hexa­aqua­(μ2-fumarato-κ4 O 1,O 1′:O 4,O 4′)bis­(μ3-maleato-κ4 O 1,O 1′:O 4:O 4′)disamarium(III)] hexa­hydrate]

Bao Li; Li-Xin Wu

doi:10.1107/S1600536810045204

. 2010 Nov 10;66(Pt 12):m1540. doi: 10.1107/S1600536810045204

Poly[[hexaaqua(μ₂-fumarato-κ⁴ O ¹,O ^1′:O ⁴,O ^4′)bis(μ₃-maleato-κ⁴ O ¹,O ^1′:O ⁴:O ^4′)disamarium(III)] hexahydrate]

Bao Li ^a, Li-Xin Wu ^a,^*

PMCID: PMC3011504 PMID: 21589236

Abstract

In the title coordination polymer, {[Sm₂(C₄H₂O₄)₃(H₂O)₆]·6H₂O}_n, the Sm^III ion is nine-coordinated by four O atoms from three different maleate ligands, two O atoms from one fumarate ligand and three O atoms from three water molecules. The fumarate ligand lies on an inversion center. Adjacent Sm^III ions are bridged by the maleate and fumarate ligands, forming a layer parallel to (011). The layers are further linked by intermolecular O—H⋯O hydrogen bonds into a three-dimensional supramolecular network.

Related literature

For the structures of transition metal complexes with malonate ligands, see: Li et al. (2006 ▶); Ye et al. (2007 ▶); Zhu et al. (2007 ▶). For a related structure, see: Hansson & Thörnqwist (1975 ▶).

Experimental

Crystal data

[Sm₂(C₄H₂O₄)₃(H₂O)₆]·6H₂O
M _r = 859.08
Triclinic,
a = 6.150 (3) Å
b = 10.679 (6) Å
c = 11.214 (6) Å
α = 69.99 (3)°
β = 79.64 (2)°
γ = 89.74 (2)°
V = 679.4 (6) Å³
Z = 1
Mo Kα radiation
μ = 4.38 mm⁻¹
T = 290 K
0.08 × 0.07 × 0.06 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.732, T _max = 0.782
6707 measured reflections
3071 independent reflections
2950 reflections with I > 2σ(I)
R _int = 0.018

Refinement

R[F ² > 2σ(F ²)] = 0.017
wR(F ²) = 0.066
S = 1.00
3071 reflections
172 parameters
H-atom parameters constrained
Δρ_max = 0.58 e Å⁻³
Δρ_min = −0.58 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: PLATON (Spek, 2009 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810045204/hy2363sup1.cif

e-66-m1540-sup1.cif^{(16.5KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810045204/hy2363Isup2.hkl

e-66-m1540-Isup2.hkl^{(150.7KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7B⋯O6ⁱ	0.85	1.88	2.680 (4)	156
O7—H7A⋯O11ⁱⁱ	0.85	1.95	2.774 (5)	164
O8—H8A⋯O11ⁱⁱⁱ	0.85	1.94	2.770 (5)	164
O8—H8B⋯O10ⁱⁱ	0.85	1.97	2.792 (5)	164
O9—H9A⋯O7^iv	0.85	2.10	2.893 (4)	155
O9—H9B⋯O3^iv	0.85	1.97	2.808 (4)	168
O10—H10A⋯O1^v	0.85	1.97	2.783 (4)	160
O10—H10B⋯O12	0.85	1.95	2.761 (5)	159
O11—H11B⋯O12	0.85	1.93	2.775 (5)	171
O11—H11A⋯O10^iv	0.85	1.95	2.755 (5)	157
O12—H12A⋯O4^vi	0.85	1.87	2.705 (5)	168
O12—H12B⋯O5ⁱⁱ	0.89	1.98	2.744 (5)	142

Open in a new tab

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

Acknowledgments

This work was supported financially by the National Basic Research Program of China (grant No. 2007CB808003) and the National Natural Science Foundation of China (grant Nos. 20973082, 20921003, 20703019).

supplementary crystallographic information

Comment

Diacids have been widely used to form metal–organic frameworks. Recently, we reported several compounds based on malonate ligand and different transition metal ions (Li et al., 2006; Ye et al., 2007; Zhu et al., 2007). Hererin, we report the crystal structure of the title compound based on maleate ligand.

The structure of the title compound is shown in Fig. 1. The bond lengths and angles are normal and comparable with those reported for a similar structure (Hansson & Thörnqwist, 1975). The Sm^III ion is nine-coordinated by four O atoms from three maleate ligands, two O atoms from one fumarate ligand and three coordinated water molecules. The two carboxylate groups of the fumarate ligand and one of the carboxylate groups of the maleate ligand exhibit a chelating coordination mode, while the other carboxylate group of the maleate ligand binds Sm^III ions in a bidentate bridging mode. Adjacent Sm^III ions are bridged by the maleate and fumarate ligands, forming a layer parallel to (0 1 1) (Fig. 2). Additionly, abundant O—H···O hydrogen bonds stabilize the crystal structure of the title compound (Table 1).

Experimental

Maleic acid and Sm(NO₃)₃ of analytical grade are used without further purification. Sm(NO₃)₃ (67.24 mg, 0.2 mmol) and maleic acid (69.64 mg, 0.6 mmol) were dissolved in water (10 ml), and the pH value was adjusted to about 3 using a dilute NaOH solution. The mixture was stirred for half an hour and then filtered. The filtrate was allowed to stand at room temperature for two weeks, giving colorless block-shaped crystals.