Synthesis, structure refinement and characterization of tetrahydrated acid gadolinium diphosphate HGdP2O7·4H2O

Synthesis and single crystal structure are reported for a new gadolinium acid diphosphate tetrahydrate HGdP2O7·4H2O. This salt crystallizes in the monoclinic system, space group P21/n, with the following unit-cell parameters: a = 6.6137(2) Å, b = 11.4954(4) Å, c = 11.377(4) Å, β = 87.53(2)° and Z = 4. Its crystal structure was refined to R = 0.0333 using 1783 reflections. The corresponding atomic arrangement can be described as an alternation of corrugated layers of monohydrogendiphosphate groups and GdO8 polyhedra parallel to the ( 1 ¯   0   1 ) plane. The cohesion between the different diphosphoric groups is provided by strong hydrogen bonding involving the W4 water molecule. Raman spectra of HGdP2O7·4H2O confirm the existence of the characteristic bands of diphosphate group in 980–700 cm−1 area. The IR spectrum reveals also the characteristic bands of water molecules vibration (3600–3230 cm−1) and acidic hydrogen ones (2340 cm−1). TG and DTA investigations show that the dehydration of this salt occurs between 79 and 900 °C. It decomposes after dehydration into an amorphous phase. Gadolinium diphosphate Gd4(P2O7)3 was obtained by heating HGdP2O7·4H2O in a static air furnace at 850 °C for 48 h.