A new vanadium(Ⅲ) phosphite [V 2(HPO 3) 3(H 2O) 3]·H 2O was synthesized hydrothermally by using V 2O 5, H 3PO 3 and triethylamine as the reactants. The as-synthesized product was characterized by powder X-ray diffraction, IR spectroscopy and ICP analysis. The result of single-crystal X-ray diffraction analysis shows that the title compound crystallized in the monoclinic space group P2 1(No.4) with the parameters a=0.783 9(2) nm, b=1.020 6(3) nm, c=0.824 7(2) nm, β= 112.510(4)°, V= 0.609 6(3) nm 3, Z=2. Its structure is built up by alternation of octahedral VO 5(H 2O), VO 4(H 2O) 2 and pseudo-pyramidal HPO 3 units to generate a three-dimensional framework structure where there exist water molecules.
The title compound [Zn(Py) 2L] n(L=1,2′-ferrocenedicarboxylate) was synthesized under mild conditions and its crystal structure was characterized. It crystallizes in a monoclinic system, space group C2/c with the cell parameters a=1.683 0(5) nm, b=1.380 4(3) nm, c=1.746 2(3) nm, β=108.78(2)°, V=3.840 8(15) nm 3, Z=8, M r=485.52, T=293(2) K, D c=3.359 Mg/m 3, μ= 4.073 mm -1, F(000)=3 872, R 1=0.040 1, wR 2=0.113 2. The compound exhibits an unusual one-dimensional chain consisting of two zigzag chains.
A new zinc hydrogen phosphite C4H8N2H4·Zn（HPO3）2 was prepared by hydrothermal method in the presence of piperazine as a structure-directing agent and the crystal structure was determined by single-crystal X-ray diffraction analysis and further characterized by X-ray powder diffraction, IR, ICP, elemental analysis and TG analysis. This compound has one-dimensional anionic chains containing four-membered rings built from corner-sharing linked alternating ZnO4 tetrahedra and HPO3 pseudo pyramids. The zinc hydrogen phosphite chains are interacted with the templates of diprotonated piperazine by N—H…O hydrogen bond. Crystal data for C4H8N2H4·Zn（HPO3）2∶monoclinic, space group C2/c. a=1.774 8（2） nm, b=0.724 28（9） nm, c=0.880 87（11） nm, β= 105.345（3）°, V=1.091 9（2） nm 3, Z=4, Dc=1^907 Mg/m 3, R1=0.022 9, wR2=0.058 8.
