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The synthesis and structures of two new compounds with the general formula N(C2H4NH3)3(H2TO4)(HTO4)·2H2O (T = P, As) are reported. They crystallize with triclinic unit cells and are isotropic. We determined the structure of phosphate salt. The following unit cell parameters were found: a = 9.886(4), b = 9.308(2), c = 10.140(3) Å, α = 109.38(2), β = 108.83(3), γ = 74.40(3)°, V = 819.2(5) Å3, and ρcal. = 1.537 g · cm−3. The crystal structure was solved with a final R = 0.042 for 3748 with I > 3σ I). The space group is P-1 and Z = 2. The atomic arrangement can be described as a three-dimensional network of hydrogen bonds made up from HnPO4 3−n (n = 1, 2) anions and H 2 O molecules between which are trapped the tris(2-ammoniumethyl)amine cations. Solid-state 13C and 31P MAS-NMR spectroscopies are in agreement with X-ray structure. Ab initio calculations allow the attribution of the phosphorus signals to the independent crystallographic sites.
Acknowledgments
We would like to thank the Secretary of State for Scientific Research and Technology of Tunisia for its financial support.
Crystallographic Data for the structure reported in this article have been deposited into the Cambridge Crystallographic Data Center as supplementary publication No. 260135. Copies of the data can be obtained, free of charge, on application to the CCDC, 12 Union Road, Cambridge CB 12EZ, UK. E-mail: [email protected].
