Crystal Structure of Poly [(4, 5-Imidazoledicarboxylato) Lead (II

Ζ. Kristallogr. NCS 224 (2009) 481-482 / DOI 10.1524/ncrs.2009.0209 481 © by Oldenbourg Wissenschaftsverlag, München

Crystal structure of poly[(4,5-imidazoledicarboxylato)lead(II)],

[Pb3(Cl0H2N4O8)]n

Zhan-Lin Xu*·1, Xiu-Mei Lin and Qing-Wei Wang1

1 Jilin Normal University, Department of Chemistry, Siping, Jilin 136000, P. R. China " Tonghua Teachers College, Department of Chemistry, Tonghua, Jilin 134002, P. R. China

Received May IS, 2009, accepted and available on-line June 24,2009; CCDC no. 1267/2658

open frameworks [6,7]. The architectures of MOFs or supramolecular compounds constructed from Pb(II) and H3IDC have rarely been reported to date [8]. The title struture possesses a 3D architecture in which the asym- metric unit contains three Pb atom and two crystallographically unique IDC ligands. The Pbl is four-coordinated with two Ν atoms (d(Pbl—Nl) = 2.326(5) Â, d(Pbl—NIA) = 2.326(5) A) and two O atoms (d(Pbl—02) = 2.455(4) Λ,

CioH2N408Pb3, monoclinic, C\2Jc\ (no. 15), a = 22.853(2) Â, [010]. b = 4.7321(4) Â, c = 14.450(1) Α, β = 113.912(1)°, V = 1428.6 Â3, Ζ = 4, RgJF) = 0.016, wR^F2) = 0.033, Table 1. Data collection and handling. 7=273 Κ. Crystal: colorless block, size 0.06 χ 0.06 χ 0.06 mm Source of material Wavelength: Mo Ka radiation (0.71073 Â) 1 A mixture of Pb(N03)2 (0.5 mmol, 0.165 g), 4,5-imidazole- μ· 353.23 cm" dicaroxylic acid (H3IDC, 0.5 mmol, 0.085 g), 2,2-bipyridine Difiractometer, scan mode: Bruker ΑΡΕΧΠ CCD, φ/ω 20max: 51° (0.5 mmol, 0.078 g) and H2O ( 18 mL) in a 30 mL Teflon-lined au- N(hkl)mtasimi, N(hkl}umque· 3627,1310 toclave under autogenous pressure at 423 Κ for five days. After Criterion for /obs, N(hkl)gi. /obs > 2 o(Iobs), 1257 cooling to room temperature, colorless block-like crystals were N(param)nfweA'· 115 collected by filtration and washed with distilled water (yield Programs: SHELXS-97 [9], SHELXL-97 [10], SHELXTL [11] 42 %).

Discussion Table 2. Atomic coordinates and displacement parameters (in Â2). Lead is a toxic metal, so the study of Pb(II) model complexes in biological systems and removal of lead by chelating agents Atom Site χ y ζ Uiso through coordination is very important [1]. Lead(II) possesses a large radius, avariable stereochemical activity, and a flexible co- H(l) 8/ 0.4385 0.0696 0.9103 0.022 ordination environment, which provides unique opportunities for the construction of novel metal-organic frameworks (MOFs) [2]. Imidazole-4,5-dicarboxylic acid is a kind of multidentate N- or O-donor ligand that can be deprotonated to generate Η2ΠΧΖΓ, HIDC2-, and IDC3- anions, dependent on the pH level, and hence may result in a large diversity of molecular or supramolecular architectures. However, most of the work has so far focused on the assembly of the d-block [3-5] or the lanthanides metal-organic

* Correspondence author (e-mail: [email protected]) 482 [Pb3(CioH2N408)]„

Table 3. Atomic coordinates and displacement parameters (in Â2).

Atom Site X y ζ Uu U22 I/33 Un Un Un

Pb(l) 4« Vi 0.43941(6) V* 0.0101(2) 0.0074(2) 0.0368(2) 0 0.0072(2) 0 Pb(2) 8/ 0.30212(1) 0.36347(4) 0.39683(2) 0.0125(2) 0.0075(1) 0.0090(1) -0.00021(7) 0.0039(1) -0.00039(7) C(l) 8/ 0.4178(3) 0.006(1) 0.8440(5) 0.025(4) 0.011(3) 0.023(3) -0.007(3) 0.013(3) -0.004(2) C(2) 8/ 0.3539(2) -0.226(1) 0.7138(4) 0.005(3) 0.013(3) 0.005(3) 0.000(2) -0.002(2) -0.003(2) C(3) 8/ 0.3911(3) -0.048(1) 0.6837(4) 0.008(3) 0.006(2) 0.007(3) -0.001(2) 0.001(2) -0.004(2) C(4) 8/ 0.3036(3) -0.436(1) 0.6605(4) 0.014(3) 0.009(2) 0.003(2) 0.002(2) -0.001(2) 0.002(2) C(5) 8/ 0.3905(3) 0.045(1) 0.5849(4) 0.012(3) 0.010(2) 0.012(3) 0.006(2) 0.004(2) 0.005(2) N(l) 8/ 0.4316(2) 0.1002(9) 0.7679(4) 0.013(3) 0.013(2) 0.013(3) -0.002(2) 0.006(2) -0.001(2) N(2) 8/ 0.3716(2) -0.187(1) 0.8159(3) 0.015(3) 0.020(2) 0.010(2) -0.005(2) 0.003(2) -0.003(2) CKD 8/ 0.3493(2) -0.0523(8) 0.5029(3) 0.023(3) 0.011(2) 0.015(2) 0.005(2) 0.010(2) 0.004(2) 0(2) 8/ 0.4306(2) 0.2318(8) 0.5864(3) 0.007(2) 0.019(2) 0.023(2) 0.003(2) 0.006(2) 0.010(2) 0(3) 8/ 0.2981(2) -0.5517(8) 0.5810(3) 0.022(3) 0.018(2) 0.013(2) -0.004(2) 0.011(2) -0.004(2) 0(4) 8/ 0.2681(2) -0.5011(8) 0.7067(3) 0.017(2) 0.022(2) 0.015(2) -0.014(2) 0.010(2) -0.008(2)

Acknowledgment, lilis work was supported by Science and Technology Re- search Projects of China (grant no. 2007.213).

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