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Piperazinium dihydrogen phosphate,C4H12N2(H2PO4)2: Synthesis, 31P CP/MAS NMR,structural and thermal investigations
Affiliation:1. Interdisciplinary Nanoscience Center (iNANO), Department of Chemistry, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C, Denmark;2. Instrument Centre for Solid-State NMR Spectroscopy (iNANO), Department of Chemistry, University of Aarhus, DK-8000 Aarhus C, Denmark
Abstract:A new piperazinium dihydrogen orthophosphate, C4H12N2(H2PO4)2 was discovered and characterized by combining information from X-ray diffraction, 31P CP/MAS NMR and thermal analysis (TG/DTA). The compound C4H12N2(HPO4)·H2O, was also studied in order to compare these two similar materials. The hydrothermal stability is investigated for the system: 1.0 C4H10N2: n H3PO4: 55–60 H2O, 0.5 < n < 3. The reaction mixtures with pH in the range 1.6–8.4 were placed at a fixed temperature in the range 20–180 °C for ca. 5 days. C4H12N2(H2PO4)2 was obtained when n > ca. 2. A crystal of piperazinium dihydrogen phosphate, C4H12N2(H2PO4)2 was structurally investigated using X-ray diffraction: triclinic, space group P1¯, a = 7.023(2), b = 7.750(3), c = 12.203(4) Å, α = 84.668(7), β = 81.532(7) and γ = 63.174(6)°, V = 586.0(4) Å3 and Z = 2. The reactivity of C4H12N2(H2PO4)2 was investigated by systematic solvothermal syntheses.
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