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Sonochemical Synthesis and Characterization of the New Micro-Hexagonal-Rod Lead (II)-Azido Coordination Compound

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Abstract

The preparation of micro hexagonal-rods of a new 1D polymeric lead(II) complex containing the Pb2-(μ-N3)2 motif, [Pb(dmp)(N3)2] n (dmp is the abbreviation of 2,9-dimethyl-1,10-phenanthroline) by the sonochemical method is described. The new microcrystal is characterized by scanning electron microscopy, X-ray diffraction (XRD), elemental analyses and infrared spectroscopy. A single crystalline material is obtained by applying a heat gradient applied to a solution of the reagents. The single-crystal XRD analyses show that the coordination number for the Pb(II) ions is six, PbN6, with “stereo-chemically active” electron lone pairs and the coordination sphere being hemidirected. The single-crystal X-ray data show the chains of [Pb(dmp)(N3)2] n interact with each other through the π–π stacking interactions, which create a 3D framework.

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Scheme 1
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Notes

  1. Crystal data 1: C28H24N16Pb2, M r  = 999.01, triclinic, space group Pī, a = 6.7056(4), b = 11.1241(2), c = 11.4224(3) Å, α = 117.979(1)°, β = 99.642(1), γ = 95.816(1), V = 725.80(5) Å3, Dc (Z = 1 f.u.) = 2.286 Mg/m3, F(000) = 468. Specimen: 0.65 × 0.25 × 0.08 mm3; R(wR) = 0.0486 (0.0829) for 6,288 reflections with I > 2σ(I).

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Acknowledgments

This work is funded by the World Class University Grant R32-2008-000-20082-0 of the National Research Foundation of Korea.

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Authors and Affiliations

  1. WCU Nano Research Center, Yeungnam University, Gyeongsang, 712-749, Korea

    Younes Hanifehpour, Babak Mirtamizdoust & Sang Woo Joo

  2. Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran

    Younes Hanifehpour & Babak Mirtamizdoust

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  1. Younes Hanifehpour
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  2. Babak Mirtamizdoust
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Correspondence to Sang Woo Joo.

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Hanifehpour, Y., Mirtamizdoust, B. & Joo, S.W. Sonochemical Synthesis and Characterization of the New Micro-Hexagonal-Rod Lead (II)-Azido Coordination Compound. J Inorg Organomet Polym 22, 916–922 (2012). https://doi.org/10.1007/s10904-012-9681-0

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