25758-26-3Relevant articles and documents
High-Pressure Metathesis of the M 1- xPO3+4 xN1-4 x (x ≈ 0.05) and M 0.75PO4 (M = Zr, Hf) Orthophosphates
Klo?, Simon D.,Weis, Andreas,Wandelt, Sophia,Schnick, Wolfgang
, p. 4164 - 4170 (2018/04/06)
We describe the oxonitridophosphates M1-xPO3+4xN1-4x (x -0.05) and the isotypic oxophosphates M0.75PO4 (M = Zr, Hf) obtained by high-pressure metathesis. The structures (ZrSiO4-type, space group I41/amd (no. 141), a = 6.5335(7)-6.6178(12), c = 5.7699(7)-5.8409(9) ?, Z = 4) were refined from single-crystal X-ray diffraction data, and the powder samples were examined with quantitative Rietveld refinement. Infrared spectroscopy did not indicate the presence of X-H (X = O, N) bonds. The optical band gaps, between 3.5 and 4.3 eV, were estimated from UV-vis data using the Kubelka-Munk function under assumption of a direct band gap. Temperature-dependent powder X-ray diffraction showed a phase transformation of the M0.75PO4 (M = Zr, Hf) compounds to ambient pressure polymorphs at 780 (Zr) and 900 °C (Hf). The preparation of the nitrogen containing compounds exemplifies the systematic access to the new class of group 4 nitridophosphates granted by high-pressure metathesis. Moreover, we show that high-pressure metathesis can also be used for the preparation of metastable oxophosphates.
Li14(PON3)2O - A non-condensed oxonitridophosphate oxide
Baumann, Dominik,Schnick, Wolfgang
, p. 617 - 621 (2015/02/19)
Li14(PON3)2O was synthesized by reaction of phosphoric triamide PO(NH2)3 with LiNH2 at 550 °C. It crystallizes in a trigonal structure [P3ˉ (no. 147), a = 5.6880(5), c = 8.0855(8) ?, V = 226.55(5) ?3, Z = 1] that can be described as a defect variant of the antifluorite structure type. The crystal structure was elucidated from X-ray powder diffraction data and corroborated by FTIR and solid-state NMR spectroscopy. Li14(PON3)2O is composed of non-condensed PON36- tetrahedra and O2- ions that are surrounded by tetrahedrally coordinated Li+. This is the first example of an ortho-oxonitridophosphate.
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 (2012/04/17)
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.
Functionalized ionic liquids, and methods of use thereof
-
, (2008/06/13)
One aspect of the present invention relates to ionic liquids comprising a pendant Bronsted-acidic group, e.g., a sulfonic acid group. Another aspect of the present invention relates to the use of an ionic liquid comprising a pendant Bronsted-acidic group to catalyze a Bronsted-acid-catalyzed chemical reaction. A third aspect of the present invention relates to ionic liquids comprising a pendant nucleophilic group, e.g., an amine. Still another aspect of the present invention relates to the use of an ionic liquid comprising a pendant nucleophilic group to catalyze a nucleophile-assisted chemical reaction. A fifth aspect of the present invention relates to the use of an ionic liquid comprising a pendant nucleophilic group to remove a gaseous impurity, e.g., carbon dioxide, from a gas, e.g., sour natural gas.
Polymeric phosphoramides
-
, (2008/06/13)
Polymeric phosphoramides -- these are illustrated by polymeric phosphoramides of the formula unit STR1 where OA is an oxirane derived unit, n is a number and N is an amine moiety; and to uses thereof.
Pentavalent phosphorus amides of cephalosporins and separation process using same
-
, (2008/06/13)
Novel pentavalent phosphorus amide derivatives of cephalosporin compounds having an amino group substituent (e.g., diethylphosphoramide of cephalosporin C) and a process for recovery of such cephalosporin compounds wherein the pentavalent phosphorus derivatives thereof are extracted with cyclohexanone, and, if desired, precipitated as cyclohexylamine salts.