The vanadyl oxalatophosphates (C 2 H 10 N 2 )[VO(HPO 4 )] 2 (C 2 O 4 ), 1, and (CH 6 N 3 ) 2 [VO(HPO 4 )] 2 (C 2 O 4 ), 2, have been synthesized hydrothermally and characterized by a combination of techniques including infrared spectroscopy, single-crystal/powder X-ray diffraction, scanning/transmission electron microscopy, thermogravimetric analysis, and magnetic susceptibility measurements. The structures of 1 and 2 contain the same type of {[VO(HPO 4 )] 2 (C 2 O 4 )} 2 - layer, including both oxalate and phosphate anions coordinated to vanadium cations, as found in the previously reported (NH 4 ) 2 [VO(HPO 4 )] 2 (C 2 O 4 )·H 2 O. Above ∼550 °C, 1 and 2 transform to (VO) 2 P 2 O 7, the catalyst for the oxidation of butane to maleic anhydride. An intermediate phase with the composition VOHPO 4 is observed in the decomposition reactions. Crystal data: ( 1 ) triclinic, space group P 1̄ (no. 2); a = 6.3595(7) Å, b = 6.6236(7) Å, c = 9.224(1) Å, α = 98.216(2) o, β = 108.128(2) o, γ = 100.672(2) o, V = 354.42(7) Å 3, Z = 1; ( 2 ) triclinic, space group P 1̄ (no . 2); a = 6.3825(8) Å, b = 7.8877(9) Å, c = 9.202(1) Å, α = 66.602(2) o, β = 71.757(2) o, γ = 79.821(2) o, V = 403.07(8) Å 3, Z = 1.
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Do et al. (2001) studied this question.
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