Chem. J. Chinese Universities

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Hydrothermal Synthesis and Characterization of Two Coordination Polymers of Flexible Acid and Lead: [Pb6(H2O)2(cit)4]·3H2O and Pb(tar)(H2O)2

SHI Jing1, XU Jia-Ning1, ZHANG Ping1*, FAN Yong1, WANG Li1, BI Ming-Hui2, MA Kui-Rong1, SONG Tian-You2*   

    1. College of Chemistry,
    2. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130012, China
  • Received:2006-12-22 Revised:1900-01-01 Online:2007-09-10 Published:2007-09-10
  • Contact: ZHANG Ping

Abstract: Two coordination polymers [Pb6(H2O)2(cit)4]·3H2O(1)(H3cit=citric acid) and Pb(tar)(H2O)2(2)(tar=tartaric acid) were synthesized under hydrothermal conditions and characterized via IR, TG-DTA, C, H, N elemental analysis, XRD and single crystal X-ray diffraction analysis. There are three Pb, two cit ligand and two free water molecules in the asymmetry unit in complex 1. The Pb ions in complex 1 coordinate to cit anions with the coordination number of 4, 5, 7 to form a neutral 3D framework. Complex 1 crystallizes in the triclinic system, space group P1 with a=0.97053(19) nm, b=0.9764(2) nm, c=1.0955(2) nm, α=109.016(3)°, β=98.380(3)°, γ=92.136(3)°, V=0.9671(3) nm3, Z=2, R1=0.0420, wR2=0.01049, GOF=1.064. In the asymmetry unit of complex 2, there are a six-coordinated Pb, a tar ligand and a water molecule. Complex 2 has a structure of extended racemic ladder-like chain, these chains are assembled by complicated H-bonds to 3D supramolecular structure. It crystallizes in the orthorhombic system, space group Pbac with a=1.39739(6) nm, b=0.64922(2) nm, c=1.80354(10) nm, V=1.63620(13) nm3, Z=8, R1=0.0283, wR2=0.0649, GOF=1.014. In both complexes 1 and 2, the α hydroxyl and α carboxyl adopt a chelate mode, and the 6s lone pair of electrons of Pb has a stereochemistry activity resulting the distribution of the bonds in a hemisphere.

Key words: Hydrothermal synthesis, Crystal structure, Lead citrate, Lead tartrate

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