Poly[μ-aqua-diaqua­(μ3-N′-carboxy­methyl­ethylenediamine-N,N,N′-tri­acetato)oxidopotassium(I)vanadium(IV)]

Rui-Hong Zhang; Li-Ping Lu; Ming-Xia Li; Miao-Li Zhu

doi:10.1107/S1600536808017030

. 2008 Jun 7;64(Pt 7):m897. doi: 10.1107/S1600536808017030

Poly[μ-aqua-diaqua(μ₃-N′-carboxymethylethylenediamine-N,N,N′-triacetato)oxidopotassium(I)vanadium(IV)]

Rui-Hong Zhang ^a, Li-Ping Lu ^a, Ming-Xia Li ^a, Miao-Li Zhu ^a,^*

PMCID: PMC2961877 PMID: 21202763

Abstract

In the crystal structure of the title compound, [KV(C₁₀H₁₃N₂O₈)O(H₂O)₃]_n, the V^IV ion adopts a distorted octahedral geometry, coordinated by one oxide group, two N and three carboxylate O atoms from the same N′-carboxymethylethylenediamine-N,N,N′-triacetate (HEDTA) ligand. The potassium ion is heptacoordinated by two water molecules, two bridging water molecules and three carboxylate O atoms from three neighbouring HEDTA ligands. The HEDTA ligands and some of the water molecules act as bridges, linking the compound into a three-dimensional architecture via 2₁ screw, c-glide, translation and inversion symmetry operators. Meanwhile, three types of O—H⋯O hydrogen bonds provide an additional stabilization of the three-dimensional architecture.

Related literature

For related literature, see: Crans et al. (2004 ▶); Khanra et al. (2007 ▶); Tsuchida et al. (1999 ▶).

Experimental

Crystal data

[KV(C₁₀H₁₃N₂O₈)O(H₂O)₃]
M _r = 449.31
Monoclinic,
a = 6.6701 (13) Å
b = 13.618 (3) Å
c = 18.693 (4) Å
β = 96.150 (2)°
V = 1688.2 (6) Å³
Z = 4
Mo Kα radiation
μ = 0.90 mm⁻¹
T = 298 (2) K
0.40 × 0.30 × 0.20 mm

Data collection

Bruker SMART 1K CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2000 ▶) T _min = 0.714, T _max = 0.840
6813 measured reflections
2957 independent reflections
2613 reflections with I > 2σ(I)
R _int = 0.024

Refinement

R[F ² > 2σ(F ²)] = 0.036
wR(F ²) = 0.088
S = 1.07
2957 reflections
236 parameters
H-atom parameters constrained
Δρ_max = 0.33 e Å⁻³
Δρ_min = −0.22 e Å⁻³

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL/PC (Sheldrick, 2008 ▶); software used to prepare material for publication: PLATON (Spek, 2003 ▶) and publCIF (Westrip, 2008 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808017030/fj2120sup1.cif

e-64-0m897-sup1.cif^{(24.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808017030/fj2120Isup2.hkl

e-64-0m897-Isup2.hkl^{(145.1KB, 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
O8—H8⋯O3ⁱ	0.82	1.75	2.542 (3)	162
O12—H12B⋯O11ⁱⁱ	0.82	2.03	2.802 (3)	157
O11—H11B⋯O4ⁱⁱⁱ	0.82	2.17	2.960 (3)	162
O10—H10B⋯O6ⁱⁱⁱ	0.82	2.20	2.987 (3)	161
O12—H12A⋯O5^iv	0.82	1.99	2.804 (3)	169
O11—H11A⋯O7ⁱⁱ	0.82	1.99	2.801 (3)	169
O10—H10A⋯O12^v	0.82	2.26	2.983 (3)	147

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

Acknowledgments

The authors acknowledge financial support from the National Natural Science Foundation of China (grant No. 20471033), the Provincial Natural Science Foundation of Shanxi Province of China (grant No. 20051013) and the Overseas Returned Scholar Foundation of Shanxi Province of China in 2006.

supplementary crystallographic information

Comment

The vanadium complexes have been attracted great attention because of their versatile properties including biological activities(Crans et al., 2004), magnetic property(Khanra et al., 2007), catalytic abilities (Tsuchida et al., 1999) and so on. Especially, we are interested in the protein tyrosine phosphatase 1B (PTP1B) inhibition activity of vanadium compounds. Thus, the title compound (I) was synthesized and its crystal structure is reported here.

The X-ray crystallographic analysis shows that there are two metal ion centres in the asymmetric unit of the title compound(Fig 1). V^IV adopts a six coordinated geometry consisting of a O atom(O1) from vanadyl, two N and three carboxyl O atoms(O2, O4 and O6) from same symmetric edta ligand while potassium is hepta-coordinated by two water molecules, two bridging water molecules and three carboxyl O atoms (O3, O5 and O9) respectively from three neighbouring edta ligands with different symmetry. Each edta ligand acts as a bridge simultaneously coordinating to three neighbouring K⁺ ions while coordinating to one vanadium. Neighbouring K⁺ ions are bridged through two coordinated water molecules(O10). As the result of these coordination, the compound is constructed to three-dimensional structure by O9 atom via 2₁-screw, O3 via c-glide & translation and K1 via inversion & translation(Fig 2). Meanwhile, three types of O—H···O hydrogen bonds (Table 1) take part in the stabilization of the three-dimensional architecture(Fig 2). The first type is the coordination water O atoms (O10, O11 and O12) acting as H donors while carboxyl O atoms(O4, O5, O6 and O7) of edta ligands as acceptors. The second is between coordination water molecules[O12—H12B···O11(-x, 2 - y, 1 - z) and O10—H10A···O12(1 + x, y, z)]. The third type of O8—H8···O3(1 - x, 2 - y, -y) hydrogen bond joins neighbouring edta ligands.

Experimental

All chemicals were of reagent grade, were commercially available and were used without further purification. H4EDTA(11.69 g, 40 mmol) was added to 100 ml of water and neutralized with 11.20 g (80 mmol) of Potassium carbonate. 6.52 g (40 mmol) of VOSO₄ was added to the solution, stirred for 24 h. Evaporation of the solution using a rotary evaporator was concentrated to 20 ml, then the solution with blue flocculent crystals was filtered, The blue crystals were obtained by slow evaporation of the solvent about two days at room temperature.