13455-05-5Relevant academic research and scientific papers
Ba6P12N17O9Br3- A column-type phosphate structure solved from single-nanocrystal data obtained by automated electron diffraction tomography
Mugnaioli, Enrico,Sedlmaier, Stefan J.,Oeckler, Oliver,Kolb, Ute,Schnick, Wolfgang
, p. 121 - 125 (2012)
Oxonitridophosphate Ba6P12N17O 9Br3 was synthesized by heating a multicomponent mixture of BaBr2, BaS, phosphoryl triamide and thiophosphoryl triamide in an evacuated and sealed silica-glass ampoule to 750 °C. Ba6P 12N17O9Br3 was obtained as the main product as a nanocrystalline powder. The crystal structure was determined ab initio on the basis of electron diffraction data acquired from a single needle-shaped nanocrystal by automated diffraction tomography. Ba 6P12N17O9Br3 crystallizes in the hexagonal space group P63/m (no. 176) with unit cell parameters a = 14.654(19), c = 8.255(9) A and Z = 2. Its structure includes triangular, column-shaped anions of ∞ 1{(P12N17O9)9-}, which are built from vertex-sharing P(O,N)4 tetrahedra with 3-rings and three-coordinate nitrogen atoms. The 1D anions are separated by Ba2+ and Br- ions, which are arranged in channels parallel to the phosphate anions along [001]. The Ba2+ ions are eight- and nine-coordinated by Br- and O/N atoms, respectively.
Unprecedented zeolite-like framework topology constructed from cages with 3-rings in a barium oxonitridophosphate
Sedlmaier, Stefan J.,Doeblinger, Markus,Oeckler, Oliver,Weber, Johannes,Schmedt Auf Der Guenne, Joern,Schnick, Wolfgang
, p. 12069 - 12078 (2011/09/16)
A novel oxonitridophosphate, Ba19P36O 6+xN66-xCl8+x (x ≈ 4.54), has been synthesized by heating a multicomponent reactant mixture consisting of phosphoryl triamide OP(NH2)3, thiophosphoryl triamide SP(NH2)3, BaS, and NH4Cl enclosed in an evacuated and sealed silica glass ampule up to 750 °C. Despite the presence of side phases, the crystal structure was elucidated ab initio from high-resolution synchrotron powder diffraction data (λ = 39.998 pm) applying the charge flipping algorithm supported by independent symmetry information derived from electron diffraction (ED) and scanning transmission electron microscopy (STEM). The compound crystallizes in the cubic space group Fm3c (no. 226) with a = 2685.41(3) pm and Z = 8. As confirmed by Rietveld refinement, the structure comprises all-side vertex sharing P(O,N)4 tetrahedra forming slightly distorted 3846812 cages representing a novel composite building unit (CBU). Interlinked through their 4-rings and additional 3-rings, the cages build up a 3D network with a framework density FD = 14.87 T/1000 A3 and a 3D 8-ring channel system. Ba2+ and Cl- as extra-framework ions are located within the cages and channels of the framework. The structural model is corroborated by 31P double-quantum (DQ) /single-quantum (SQ) and triple-quantum (TQ) /single-quantum (SQ) 2D correlation MAS NMR spectroscopy. According to 31P{1H} C-REDOR NMR measurements, the H content is less than one H atom per unit cell.
Bis(dialkylthiophosphoryl)amines as metal extractants
-
, (2008/06/13)
A process for extracting metal values especially zinc values from aqueous solutions of metal salts which comprises contacting the aqueous solution with an organic phase comprising a compound of the formula: STR1 wherein each of R1, R2/sup
Synthesis, Structure, and Thermal Behaviour of Phosphorothionic Triamide SP(NH2)3
Schnick, Wolfgang
, p. 942 - 945 (2007/10/02)
Phosphorothionic triamide SP(NH2)3 is obtained by slow addition of SPCl3 dissolved in dry CH2Cl2 to a satured solution of NH3 in CH2Cl2 at -50 deg C.Ammonium chloride is removed from the resulting precipitate by treatment with HNEt2 followed by extraction with CH2Cl2.Coarse crystalline SP(NH2)3 is obtained after recrystallization from dry methanol.The crystal structure of SP(NH2)3 has been determined by single crystal X-ray methods (Pbca; a = 922,3(1), b = 953.8(1), c = 1058.4(2) pm, Z = 8).In the crystals the molecules show non-crystallographic point symmetry Cs.The P-S bond (195,4(1) pm) is slightly longer than SPCl3.From P-N bond lengths of about 166 pm a significant electrostatic strengthening of the P-N single bonds is assumed.Weak intermolecular hydrogen bonding interactions (N-H***N>/=329,5 pm; N-H***S>/=348,3 pm) are observed.Investigations of thermal properties shows a melting temperature of 115 deg C for SP(NH2)3.According to combined DTA/TG and MS investigations above this temperature the compound decomposes by evolution of H2S and NH3 to yield amorphous phosphorus(V)nitride. - Keywords: Phosphorothionic Triamide, Synthesis, Structure, Thermal Properties
