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  • 1
    ISSN: 0044-2313
    Keywords: Phosphorus(V) nitride imide ; deuterium compound of ; synthesis of ; x-ray, synchrotron and neutron structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystalline Phosphorus(V) Nitride Imide, HPN2 and DPN2, respectively, - Structure Determination with X-Ray, Synchrotron, and Neutron RadiationMicrocrystalline HPN2 resp. DPN2 was obtained by the reaction of P3N5 with NH3 resp. ND3 in high-pressure autoclaves under ammonothermal conditions (T = 550°C, p(NH3 resp. ND3) = 6 kbar) within 14 d.
    Notes: Mikrokristallines HPN2 bzw. DPN2 entsteht bei der Umsetzung von P3N5 mit NH3 bzw. ND3 in Hochdruckautoklaven unter ammonothermalen Bedingungen (T = 550°C, p(NH3 bzw. ND3) = 6 kbar) innerhalb von 14 Tagen.Die Struktur wurde an DPN2 über Beugungsexperimente mit Synchrotron- und Neutronenstrahlung am Pulver einschließlich der D-Lagen geklärt.DPN2: P212121 (Nr. 19), a = 4,6550(2) Å; b = 4,6591(2) Å; c = 7,0560(3) Å, Z = 4, Neutronenbeugung time-of-flight: RBragg (F2o) = 0,0184, 33 Reflexe (d = 1,626 Å - d = 5,278 Å) RBragg (F2o) = 0,0218, 93 Reflexe (d = 1,080 Å - d = 2,623 Å) DPN2 ist aus allseits eckenverknüpften Tetraedern PN4/2 aufgebaut, die ein dreidimensionales Gerüst bilden, wie es unverzerrt im “idealisierten” ß-Cristobalit vorliegt. Die Deuteronen sind geordnet an die Hälfte der N-Atome gebunden.The structure was solved on DPN2 by synchrotron and neutron diffraction data including the D-positions.DPN2: P212121 (Nr. 19), a = 4.6550(2) Å; b = 4.6591(2) Å; c = 7.0560(3) Å, Z = 4, Neutron diffraction time-of-flight: RBragg(F2o) = 0.0184, 33 reflections (d = 1.626 Å - d = 5.278 Å) RBragg(F2o) = 0.0218, 93 reflections (d = 1.080 Å - d = 2.623 Å) DPN2 contains corner-sharing tetrahedra PN4/2. These form a three-dimensional network as it is observed undistorted in “idealized” ß-cristobalite. The deuterons are bonded to one half of the nitrogen atoms in an ordered way.
    Additional Material: 8 Ill.
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  • 2
    ISSN: 0044-2313
    Keywords: Ammonium diamido dioxo phosphate(V) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of an Ammonium Diamidodioxophosphate(V), NH4PO2(NH2)2The ammonolysis of P3N5 under ammonothermal conditions (T = 400°C, p(NH3) = 6 kbar, 14 d in autoclaves) in the presence of small definite amounts of water leads to the formation of NH4PO2(NH2)2. The structure was solved by single crystal X-ray methods.NH4PO2(NH2)2: P21/c (Nr. 14), a = 6.886(1) Å, b = 8.366(2) Å, c = 9.151(2) Å, β = 111.78(3)°, Z = 4, R1/wR2 = 0.026/0.072, Z(Fo2 〉 2σ(Fo2)) = 1183, N(variables) = 87. In NH4PO2(NH2)2 the anions [PO2(NH2)2]- are linked to chains by N—H … N and N—H … O bridge bonds. The ammonium ions are located between these chains and are donors for N—H … O bridge bonds which connect the chains three-dimensionally.
    Notes: Bei Ammonolysen von P3N5 unter ammonothermalen Bedingungen (T = 400°C und p(NH3) = 6 kbar 14 d in Autoklaven) führt eine geringe, definierte Menge Wasser zur Bildung von NH4PO2(NH2)2. Die Struktur wurde röntgenographisch am Einkristall bestimmt.NH4PO2(NH2)2: P21/c (Nr. 14), a = 6,886(1) Å, b = 8,366(2) Å, c = 9,151(2) Å, β = 111,78(3)°, Z = 4, R1/wR2 = 0,026/0,072, Z(Fo2 〉 2σ(Fo2)) = 1183, Z(Variable) = 87. In NH4PO2(NH2)2 sind Anionen [PO2(NH2)2]-, über N—H … N und N—H … O Brückenbindungen zu unendlichen Ketten verknüpft. Die Ammoniumionen liegen zwischen den Ketten und wirken als Donatoren für N—H … O Brückenbindungen, die die Ketten dreidimensional verknüpfen.
    Additional Material: 7 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 429-433 
    ISSN: 0044-2313
    Keywords: Potassium nitridophosphate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of a Potassium Nitridophate, K3P6N11Single phase microcrystalline K3P6N11 was obtained by the reaction of P3N5 KNH2 in supercritical ammonia (6 kbr, 500°C) after 7 d reaction time in autoclaves. The structure was solved by X-ray powder diffraction methods. K3P6N11: P4132, a = 10.388(3) Å, Z = 4, RBragg (F02) = 0.087, 51 reflections K3P6N11 contains two- and three-fold corner-sharing tetrahedra PN4. These form a three-dimensional framework with potassium in voids coordinated by (2 + 6) N for K(1) and (3 + 3 + 3) N for K(2).
    Notes: Röntgenographisch phasenreines mikrokristallines K3P6N11 entsteht bei der Umsetzung von P3N5 mit KNH2 in Ammoniak unter ammonothermalen Bedingungen (6kbar, 500°C) nach 7d Reaktionszeit in Autoklaven. Die Struktur konnte über eine Röntgenstrukturanalyse am Pulver geklärt werden. K3P6N11: P4132, a = 10,388(3) Å, Z = 4, RBragg (F02) = 0,087, 51 Reflexe K3P6N11 ist aus zweifach- und dreifach eckenverknüpften Tetraedern PN4 aufgebaut, die ein dreidimensionales Gerüst bilden, in dessen Hohlräumen die Kaliumionen K(l) von (2 + 6) N von K(2) von (3 + 3 + 3) N umgeben sind.
    Additional Material: 4 Ill.
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  • 4
    ISSN: 0044-2313
    Keywords: Cesium Diamidodioxophosphate ; synthesis ; X-ray structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of a Cesium Diamidodioxophosphate, CsPO2(NH2)2Colourless crystals of CsPO2(NH2)2 with the shape of platelets were obtained by the reaction of P3N5 with CsNH2 and CsOH · 3H2O in a molar ratio of 2:3:3 in supercritical ammonia at 400°C and p(NH3) = 6 kbar in a high-pressure autoclave within 10 days. The X-ray structure determination was successful including the positions of hydrogen.CsPO2(NH2)2: P43212 (No. 96), a = 5.630(1) Å, c = 15.320(3) Å, Z = 4, R1/Rw = 0.025/0.057 N(Fo2 〉 2σ(Fo2)) = 1309, N(Var.) = 36.P as the centres of tetrahedra - [PO2(NH2)2]- - form together with Cs the motif of a distorted NaCl type. This arrangement contains a three-dimensional network of hydrogen bridge bonds N-H … O and N-H … N.
    Notes: Farblose Kristalle von CsPO2(NH2)2 mit plättchenförmigem Habitus entstehen bei der Umsetzung von P3N5 mit CsNH2 und CsOH · 3H2O im molaren Verhältnis 2:3:3 in überkritischem Ammoniak bei 400°C und p(NH3) = 6 kbar in einem Hochdruckautoklav innerhalb von 10 Tagen. Die Struktur wurde röntgenographisch einschließlich der H-Lagen geklärt.CsPO2(NH2)2: P43212 (Nr. 96), a = 5,630(1) Å, c = 15,320(3) Å, Z = 4, R1/Rw = 0,025/0,057 N(Fo2 〉 2σ(Fo2)) = 1309, N(Var.) = 36.P als Schwerpunkte von Tetraedern - [PO2(NH2)2]- - bildet zusammen mit Cs das Motiv eines verzerrten NaCl-Typs. Zwischen den Tetraedern liegt ein dreidimensionales Netz, aus N-H … O- und N-H … N-Wasserstoff-Brückenbindungen vor.
    Additional Material: 6 Ill.
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