Hydrothermal Synthesis and Crystal Structure of an Organically Templated Open-Framework Vanadium Phosphate: (H3NCH2CH2NH3)4[VIII(H2O)2(VIVO)6(OH)2(HPO4)3(PO4)5].cntdot.3H2O
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An ethylenediamine encapsulated open-framework vanadium phosphate, (H3NCH2CH2-NH3)4[VIII(H2O)2(VIVO)6(OH)2(HPO4)3(PO4)5]•3H2O (1) has been synthesized from the hydrothermal reaction of V2O5:H3PO4:H2NCH2CH2NH2:H2O in a mole ratio of 1:6.9:3.6:265 at 170 °C for 5 days, and its structure determined by single-crystal X-ray crystallography. Phosphate 1 is monoclinic, space group C2/c, a = 20.674 (2) Å, b = 9.956 (2) Å, c = 23.694 (1) Å, α = 101.154 (5) Å. Z = 4, V = 4784.8 (10) Å3. Refinement with 3757 observed reflections for which I ≥ 3σ(I) gave R = 0.039 and Rw = 0.040. The structure consists of layers built from V(IV) square pyramids and µ2-OH bridged V(IV) pyramids with (HPO4)2- and (PO4)3- tetrahedra connected together by V(III) octahedra to give rise to the formation of very large interconnected tunnels parallel to the b axis and  direction. The tunnels are occupied by ethylenediammonium and water molecules. © 1995, American Chemical Society. All rights reserved.
author list (cited authors)
Zhang, Y., Clearfield, A., & Haushalter, R. C.