Synthesis and Characterization of Two New Compounds: N(C 2 H 4 NH 3 ) 3 (H 2 TO 4 )(HTO 4 )·2H 2 O (T = P, As).

The synthesis and structures of two new compounds with the general formula N(C 2 H 4 NH 3 ) 3 (H 2 TO 4 )(HTO 4 )·2H 2 O (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, a = 109.38(2), ß = 108.83(3), ? = 74.40(3)°, V = 819.2(5) Å 3 , and ? cal. = 1.537 g · cm -3 . The crystal structure was solved with a final R = 0.042 for 3748 with I > 3s 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 H n PO 4 3- n (n = 1, 2) anions and H 2 O molecules between which are trapped the tris(2-ammoniumethyl)amine cations. Solid-state 13 C and 31 P 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. [ABSTRACT FROM AUTHOR]