Source of materialHydrothermal reactions were carried out in 23 ml Teflon-lined stainless steel vessels at 150°Cf or 2d .P iperazine (0.086 g, 1.0 mmol), telluric acid (0.690 g, 3.0 mmol), WO 3 (0.696 g, 3mmol) and H 2O(3ml) were allowed to react. The pH values of the reaction mixture before and after the reaction were~9 and~7, respectively. The solid products were recovered by vacuum filtration and washed with water. Colorless polyhedral crystals suitable for X-ray analysis were obtained. Experimental detailsHydrogen atoms associated with the piperazinium cations were placed geometrically and refined as riding. The hydrogen atoms of lattice water molecules were not located because of the large displacement parameters of oxygen atoms. DiscussionThe crystal structure of the title compound comprises discrete centrosymmetric heteronuclear [TeW 6O24] 6-anions, doubly protonated piperazinium cations and lattice water molecules. The Anderson-Evans type [TeW 6O24]6-cluster anions is formed by close packing of oxygen atoms with tellurium and tungsten atoms in octahedral sites. The Te atom occupying the inversion center is coordinated by oxygen atoms in an early regular octahedral manner with adistances of 1.916 (4) 6-anions, piperazinium cations or to each other in acomplex arrangement.
C 10 H 18 NO 4 P, orthorhombic, Aba2(no. 41), a =7.218(1) Å, b =36.600(7) Å, c =9.188(2) Å, V =2427.2 Å 3 , Z =8, R gt (F) =0.043, wR ref (F 2 ) =0.105, T =296 K. Source of materialAhydrothermalreaction was carried out in a23mlTeflon-lined stainless steel Parr hydrothermalreaction vessel at 150°C for 2d. Phosphoric acid (0.03 ml, 0.5 mmol), 4-phenyl-butylamine (0.24 ml, 1.5 mmol), and water (3.0 ml) were allowed to react. The pH value of the solution before and after the reaction was 11.3 and 7.5, respectively. Thesolid products were recovered by vacuum filtration and washedwith water. Colorless platy crystals suitable for analysis were obtained. The yield of the crystalline product was~40 %based on phosphorous. Experimental detailsHydrogen atomswere placed in calculated positions and refined as riding except those of the hydroxylg roup in H 2 PO 4 -which werelocated in differenceFouriermaps, and their positions and isotropic displacement parameters were refined. The Flack parameter was -0.03(15). DiscussionThe KH 2 PO 4 (KDP) family is one of the most important classes in non-linear optics and ferroelectrics due to its non-centrosymmetric structure [1,2]. Many KDP analogues have been reported, and the arrangement of H 2 PO 4 -can be controlled by the species of counter cations incorporated in the structure [3][4][5][6][7]. A hydrogen bond between the counter cations and dihydrogenphosphate anions is ak ey variable to construct an oncentrosymmetric array of H 2 PO 4 -with very shortO×××Odistances.The title crystal structure is built up from a4-phenylbutylammonium cation and ad ihydrogenphosphate anion. The detailed analysis of H 2 PO 4 -confirms thepositions of oxo-andhydroxyl groups by comparing the bond distances and angles, i.e., d(P-O) of 1.4942(2) Åa nd 1.5369(3) Åa re shorter than d(P-OH) of 1.5396(2) Åand 1.5647(2) Å, and ÐO-P-O =114.2(2)°is wider than ÐHO-P-OH =109.0(1)°. Each anion H 2 PO 4 -is strongly hydrogen bonded to one another forming "macroanionic" layers perpendicular to [010]
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