K(VVO(H2O))(VIVO)O{O3P–(CH2)2–PO3}
(labelled MIL-3K) is a vanado-ethylenediphosphonate whose previously reported hybrid framework reversibly dehydrates. Its anhydrous form (KVIV/V2O3{O3P–(CH2)2–PO3} or MIL-3Kan) has been determined from X-ray powder diffraction data in the centrosymmetric triclinic P
(no. 2) space group with lattice parameters: a
= 7.2375(1) , b
= 8.1852(1), c
= 9.8862(2)
Å, α
= 83.2209(9), β
= 65.223(1), γ
= 76.492(1)°, V
= 516.90(2), Z
= 2. RF2
= 0.0920 and Rwp
= 0.0157. The two structures of MIL-3K and MIL-3Kan are quite similar, just the square pyramidal coordination of one vanadium atom of the hydrate transforms into a VVO4 tetrahedron in the dehydrated form. This change induces the opening of eight-membered channels delimited by phosphonate tetrahedra and vanadium polyhedra in strict alternation.
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