Abstract
By quenching a melt of Li4P2O7 two new, thermodynamically metastable polymorphs are obtained as biphasic mixtures. The crystal structure of one polymorph was determined from single‐crystal X‐ray diffraction data {Li4P2O7‐trig*: colorless, trigonal, P3212 (no. 153), Z = 3, a = 5.1699(2) Å, c = 18.9722(8) Å, 60 parameters, R1 = 0.018, wR2 = 0.051, 1265 unique reflections with Fo > 4σ(Fo)}. For the second polymorph a structure model was derived, using direct space methods followed by Rietveld refinement {Li4P2O7‐pseudomono*: P1, a = 7.88468(5) Å, b = 10.30394(6) Å, c = 7.54581(4) Å, α = 89.8142(6)°, β = 115.26(2)°, γ = 90.2015(5)°, RI = 7.62}. 31P‐MAS‐NMR measurements show δiso = –2.9 ppm for Li4P2O7‐pseudomono* and δiso = –6.6 ppm for the trigonal polymorph. Substitution of about 10 % lithium by copper(I) is possible in the trigonal as well as in the long known triclinic polymorph as is evidenced by the results of SXRD, XRPD, and 31P‐MAS‐NMR measurements.
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