A nine-coordinated ZrIV complex and a self-assembling system obtained from a proton transfer compound containing 2,6-pyridinedicarboxylate and 2,6-pyridinediammonium;: Synthesis and X-ray crystal structure

Starting with a zirconium salt and LH2, (pydaH(2))(2+)(pydc)(2-), (pyda=2,6-pyridinediamine; pydcH(2)=2,6-pyridinedicarboxylic acid), as a 1: 1 proton transfer self-associated compound, two different compounds were resulted. One of them is a new complex of Zr-IV with a flat pyridine containing ligand and structure of (pydaH)(2)[Zr(pydc)(3)] center dot 5H(2)O (1) and the other, (pydaH)(+)(NO3)(-) (2) is an ion pair with no zirconium ion. The zirconium(IV) complex (1) is crystallized in triclinic system with P (1) over bar space group and Z=2, the crystallographic parameters are: a=10.612(5) angstrom, b=10.617(5) angstrom, c=16.815(8) angstrom, alpha=103.654(9)degrees, beta= 95.821(9)degrees, gamma=98.891(9)degrees and R-value for 16767 collected reflections is 0.0592. The ion pair (2) has crystals of monoclinic system with P2(1) space group and Z=2. Its crystallographic parameters are: a=3.6227(11) angstrom, b= 10.034(4) angstrom, c= 10.296(4) angstrom, beta=93.422(9)degrees and R-value for 4031 collected reflections is 0.0521. The two compounds were characterized with elemental analysis, ESI/MS, NMR and IR spectroscopy.