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  • 1
    Electronic Resource
    Electronic Resource
    Chester : International Union of Crystallography (IUCr)
    Journal of synchrotron radiation 8 (2001), S. 698-700 
    ISSN: 1600-5775
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Tin nitrides (Sn3N4) prepared by the reaction of Sn-halides with KNH2 in liquid ammonia and a subsequent vacuum annealing procedure were investigated with transmission mode XAFS experiments. While the near edge data suggest the presence of a univalent Sn-compound with a valency close to +4, the analysis of the extended X-ray absorption fine structure proves the presence of two different local Sn sites in this crystal structure: While Sn(1) is surrounded by 4 nitrogen in a distance of 2.06 Å, each Sn(2) ion is coordinated with 6 nitrogen at about 2.17 Å radial distance.
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  • 2
    ISSN: 1600-5740
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: Potassium hydrogensulfide (KHS) is an ionic compound with an anionic molecular group HS^-. The fast reorientational disorder of the anions was determined for the ambient temperature modification [R\bar 3m; Jeffrey (1974). Can. J. Phys. 52, 2370–2378]. Single crystals are available now as protonated or deuterated specimens. With neutron single-crystal diffraction at room temperature, a considerable anharmonicity of the atom potential of the H or D atoms was observed. Even the thermal motions of K and S atoms show small deviations from an isotropic probability density function, which can be modelled using anharmonic temperature factors. The temperature factors of the atoms were expanded into a Gram–Charlier series [Kuhs (1992). Acta Cryst. A48, 80–98] in order to evaluate the anharmonicity quantitatively. Parameters up to a fourth-order approximation are relevant for the D atoms. Results from neutron single-crystal diffraction are compared with split-atom models extracted from neutron powder diffraction patterns of fully deuterated samples.
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  • 3
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 370 (1969), S. 248-253 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Be(NH2)2 has been prepared from the metal and ammonia at 130 to 370 °C and pressures of ammonia up to 3500 atm. Addition of a mineralizer (NaNH2) results in single crystals of the compound. It has tetragonal symmetry. The space group is I41/a2/c2/d. The lattice constants are a = 10.18, c = 16.14 Å, c/a = 1.585; Z = 32.BeNH is formed by thermal degradation of the amide in vacuum at 230 °C. The pure compound is amorphous. Berylliumimide decomposes to the nitride when heated to 250 °C.
    Notes: Be(NH2)2 wurde aus dem Metall und Ammoniak bei 130-370 °C und NH3-Drucken bis 3500 atm dargestellt. Mit Mineralisatorzusatz (NaNH2) erhält man Einkristalle der Verbindung. Sie kristallisiert tetragonal in der Raumgruppe I41/a2/c2/d. Die Gitterkonstanten sind a = 10,18, c = 16,14 Å, c/a = 1,585; Z = 32.BeNH entsteht bei der thermischen Zersetzung des Amids im Vakuum bei 230 °C. Es läßt sich rein nur röntgenamorph erhalten. Berylliumimid geht bereits bei 250 °C in Nitrid über.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 370 (1969), S. 254-261 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mg(NH2)2 was prepared by several methods. Single crystals of the compound were obtained by ammonothermal synthesis. The X-ray investigation of single crystals showed tetragonal symmetry. The lattice constants are: a = 10.37, c = 20.15 Å, c/a = 1.943; Z = 32; space group I41/a2/c2/d.MgNH was prepared by thermal decomposition of the amide at 240-365°C. Its X-ray powder diagram shows hexagonal symmetrie. The lattice constants are: a = 11.58, c = 3.677 Å, c/a = 0,318; Z = 12.On the basis of the extinctions of the X-ray powder diagram the space group with the highest possible symmetry is P6322.The volume chemistry of the amides and imides of the alkaline earth metals is discussed.
    Notes: Mg(NH2)2 wurde nach mehreren Verfahren dargestellt. Die Ammonothermalsynthese lieferte Einkristalle der Verbindung. Die röntgenographische Untersuchung mit Einkristallmethoden ergab tetragonale Symmetrie mit den Gitterkonstanten \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm a} = 10,37\,{\rm {\AA},}\quad{\rm c} = 20,15\,{\rm {\AA}}\quad{\rm und}\,{\rm c}/{\rm a} = 1,943. $$\end{document} Die Elementarzelle enthält 32 Formeleinheiten. Magnesiumamid kristallisiert in der Raumgruppe I41/a2/c2/d.MgNH läßt sich durch thermischen Abbau des Amids bei 240-365°C kristallin darstellen. Sein Pulverdiagramm wurde hexagonal indiziert. Die Gitterkonstanten sind: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm a} = 11,58\,{\rm {\AA},}\quad{\rm c} = 3,677\,{\rm {\AA}}\quad{\rm und}\,{\rm c}/{\rm a} = 0,318. $$\end{document} In der Elementarzelle befinden sich 12 Formeleinheiten. Auf Grund der Auslöschungen findet man als Raumgruppe mit der höchst möglichen Symmetrie P6322.Die Volumchemie der Erdalkalimetallamide und -imide wird diskutiert.
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  • 6
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Columnarstructures of Tri- and Diamminenitrates, [M(NH3)3]NO3 and [M(NH3)2]NO3 of Monovalent Copper and SilverIn liquid ammonia [Cu(NH3)4](NO3)2 reacts with copper at room temperature to [Cu(NH3)3]NO3; the product decomposes at lower NH3 pressures to [Cu(NH3)2]NO3. With AgNO3 single crystals of [Ag(NH3)3]NO3 can be grown from liquid NH3 and [Ag(NH3)2]NO3 from a solution of NH3 in water.Single crystal X-ray structure determination has been carried out  -  in spite of lower NH3 decomposition pressure  -  on the more stable Ag complexes. Guinier data revealed that the corresponding Cu and Ag compounds are isotypic: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm [M(NH}_{\rm 3} {\rm)}_{\rm 3}]{\rm NO}_3 :{\rm P}\mathop 6\limits^ - 2{\rm c \,N = 2} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Cu}} & {{\rm a = 7.837(2)}{\AA}} & {{\rm c = 6.036(1)}} \\\end{array}{\AA} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Ag}} & {{\rm a = 8.057(2)}{\AA}} & {{\rm c = 5.840(6)}} \\\end{array}{\AA} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {} & {{\rm R = 0.038}} & {{\rm R}_{\rm w} {\rm = 0.040}} \\\end{array}{\rm (w = 1) Z(}\mathop {\rm F}\nolimits_0^{\rm 2}) \ge 3\sigma {\rm (}\mathop {\rm F}\nolimits_0^{\rm 2}) = 217 $$\end{document} [M(NH3)2]NO3: Pnnm, N = 4 \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Cu}} & {{\rm a = 10.637(3)}{\AA}} & {{\rm b = 7.863(2)}{\AA}} & {{\rm c = 6.118(2)}{\AA}} \\\end{array} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Ag}} & {{\rm a = 10.573(2)}{\AA}} & {{\rm b = 8.110(2)}{\AA}} & {{\rm c = 6.286(1)}{\AA}} \\\end{array} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {} & {{\rm R = 0.029}} & {{\rm R}_{\rm w} {\rm = 0.033}} \\\end{array}{\rm (w = 1) Z(}\mathop {\rm F}\nolimits_0^{\rm 2}) \ge 3\sigma {\rm (}\mathop {\rm F}\nolimits_0^{\rm 2}) = 206 $$\end{document}The results of the structure determinations are given and the atomic arrangements are discussed by comparison.
    Notes: In flüssigem NH3 komproportioniert [Cu(NH3)4](NO3)2 mit elementarem Cu bei Raumtemperatur zu [Cu(NH3)3]NO3, das bei geringerem NH3-Partialdruck in die Diamminverbindung übergeht. Mit AgNO3 lassen sich aus flüssigem NH3 Kristalle von [Ag(NH3)3]NO3 und aus wäßrigem NH3 von [Ag(NH3)2]NO3 züchten.Die röntgenographische Strukturbestimmung mit Einkristallen wurde - wegen der geringeren NH3-Zersetzungsdrücke  -  an den stabileren Ag-Komplexen erfolgreich durchgeführt. Über Guinierdaten ließ sich zeigen, daß entsprechende Cu- und Ag-Verbindungen isotyp sind: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm [M(NH}_{\rm 3} {\rm)}_{\rm 3}]{\rm NO}_3 :{\rm P}\mathop 6\limits^ - 2{\rm c \,Z = 2} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Cu}} & {{\rm a = 7,837(2)}{\AA}} & {{\rm c = 6,036(1)}} \\\end{array}{\AA} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Ag}} & {{\rm a = 8,057(2)}{\AA}} & {{\rm c = 5,840(6)}} \\\end{array}{\AA} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {} & {{\rm R = 0,038}} & {{\rm R}_{\rm w} {\rm = 0,040}} \\\end{array}{\rm (w = 1) Z(}\mathop {\rm F}\nolimits_0^{\rm 2}) \ge 3\sigma {\rm (}\mathop {\rm F}\nolimits_0^{\rm 2}) = 217 $$\end{document} [M(NH3)2]NO3: Pnnm, Z = 4 \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Cu}} & {{\rm a = 10,637(3)}{\AA}} & {{\rm b = 7,863(2)}{\AA}} & {{\rm c = 6,118(2)}{\AA}} \\\end{array} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm M} \buildrel \wedge \over = {\rm Ag}} & {{\rm a = 10,573(2)}{\AA}} & {{\rm b = 8,110(2)}{\AA}} & {{\rm c = 6,286(1)}{\AA}} \\\end{array} $$\end{document} \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {} & {{\rm R = 0,029}} & {{\rm R}_{\rm w} {\rm = 0,033}} \\\end{array}{\rm (w = 1) Z(}\mathop {\rm F}\nolimits_0^{\rm 2}) \ge 3\sigma {\rm (}\mathop {\rm F}\nolimits_0^{\rm 2}) = 206 $$\end{document}.Die Ergebnisse der Strukturbestimmungen werden mitgeteilt und die Atomanordnungen vergleichend diskutiert.
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  • 7
    ISSN: 0044-2313
    Keywords: Hexaammine metal(II) halides, [M(NH3)6]X2 ; single crystal structure determinations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Structures of some Hexaammine Metal(II) Halides of 3 d Metals: [V(NH3)6]I2, [Cr(NH3)6]I2, [Mn(NH3)6]Cl2, [Fe(NH3)6]Cl2, [Fe(NH3)6]Br2, [Co(NH3)6]Br2 and [Ni(NH3)6]Cl2Crystals of yellow [V(NH3)6]I2 and green [Cr(NH3)6]I2 were obtained by the reaction of VI2 and CrI2 with liquid ammonia at room temperature. Colourless crystals of [Mn(NH3)6]Cl2 were obtained from Mn and NH4Cl in supercritical ammonia. Colourless transparent crystals of [Fe(NH3)6]Cl2 and [Fe(NH3)6]Br2 were obtained by the reaction of FeCl2 and FeBr2 with supercritical ammonia at 400°C. Under the same conditions orange crystals of [Co(NH3)6]Br2 were obtained from [Co2(NH2)3(NH3)6]Br3. Purple crystals of [Ni(NH3)6]Cl2 were obtained by the reaction of NiCl2 · 6H2O and NH4Cl with aqueous NH3 solution. The structures of the isotypic compounds (Fm3m, Z = 4) were determined from single crystal diffractometer data (see “Inhaltsübersicht”).All compounds crystallize in the K2[PtCl6] structure type. In these compounds the metal ions have high-spin configuration. The orientation of the dynamically disordered hydrogen atoms of the ammonia ligands is discussed.
    Notes: Durch Umsetzungen von VI2 und CrI2 mit flüssigem Ammoniak bei Raumtemperatur wurden gelbe Kristalle von [V(NH3)6]I2 bzw. grüne von [Cr(NH3)6]I2 erhalten. Farbloses [Mn(NH3)6]Cl2 wurde durch Umsetzung von Mn mit NH4Cl in überkritischem Ammoniak einkristallin dargestellt. Farblose und transparente Kristalle von [Fe(NH3)6]Cl2 und [Fe(NH3)6]Br2 konnten durch Umsetzung von FeCl2 bzw. FeBr2 in überkritischem Ammoniak bei 400°C erhalten werden. Wird unter den gleichen Bedingungen Tri-μ-amido-bis[triammincobalt(III)]-bromid mit Ammoniak umgesetzt, so entstehen u.a. orangefarbene Kristalle von [Co(NH3)6]Br2. Violette Einkristalle von [Ni(NH3)6]Cl2 wurden durch Umsetzung von NiCl2 · 6 H2O mit NH4Cl in wäßriger NH3-Lösung erhalten.Die Strukturen der isotypen Verbindungen [M(NH3)6]X2 (Fm3m, Z = 4) wurden aus Röntgen-Einkristall-Diffraktometerdaten bestimmt: Alle Verbindungen kristallisieren im K2[PtCl6]-Typ. Die Zentralatome liegen in den oktaedrischen Komplexen in high-spin Konfiguration vor. Die Orientierung der dynamisch fehlgeordneten Wasserstoffatome der Ammoniakliganden wird diskutiert.
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  • 8
    ISSN: 0044-2313
    Keywords: Ditetraammine lithium tetraphenyldistannide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl-Anions: The Compound [Li(NH3)4]2[Sn2Ph4]Ruby-red, brittle single crystals of [Li(NH3)4]2[Sn2Ph4] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at -35°C. The structure was determined from X-ray singlecrystal diffractometer data: Space group, P1, Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R1 (F02 ≥ 4σF02) = 5.13%, wR2 (F02 ≥ 4σF02) = 10.5%, N(F02 ≥ 4σF02) = 779, N(Var.) = 163.The compound contains to Sb2Ph4 isosteric centres [Sn2Ph4]2- as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c-plane, but stacked along [100].
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  • 9
    ISSN: 0044-2313
    Keywords: Tri-μ-amido-bis-[triammine chromium(III)]-iodide ; binuclear chromium compound ; antiferromagnetic exchange coupling ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Intramolecular Antiferromagnetism in [Cr2(μ-NH2)3(NH3)6]I3The magnetism of [Cr2(μ-NH2)3(NH3)6]I3 which consists of binuclear cations with NH2--bridged face-sharing octahedral coordination polyhedra and a metal-metal separation of 264.9 pm can be explained by antiferromagnetically exchange-coupled CrIII-3d3 pairs. The magnetochemical analysis in the temperature range 5 K - 295 K on the basis of the isotropic Heisenberg model (spin Hamiltonian Ĥ = -2 JŜ1 · Ŝ2) leads to the parameter value J = -98(3) cm-1. Compared to the exchange coupling in corresponding binuclear chromium compounds with OH- bridges and identical metal-metal separation the strength of the coupling is significantly enhanced (JNH2/JOH ≍ 1.6).
    Notes: Der Magnetismus der Zweikern-Komplexverbindung [Cr2(μ-NH2)3(NH3)6]I3, die Kationen aus zwei Chromzentrierten und über NH2--Gruppen flächenverknüpften oktaedrischen Koordinationspolyedern mit d(Cr—Cr) = 264,9 pm enthält, wird durch eine antiferromagnetische Austauschkopplung zwischen den Spins der beiden CrIII-3d3-Zentren bestimmt. Die Analyse des Temperaturverlaufs der magnetischen Suszeptibilität zwischen 5 K und 295 K auf der Grundlage des isotropen Heisenberg-Modells mit dem Spin-Hamilton-Operator Ĥ = -2JŜ1 · Ŝ2 führt zu dem Austauschparameterwert J = -98(3) cm-1. Er zeigt an, daß die antiferromagnetische Wechselwirkung gegenüber der von entsprechend aufgebauten Komplexen mit OH--Brücken und gleichem Cr—Cr-Abstand deutlich verstärkt ist (JNH2/JOH ≈ 1,6).
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  • 10
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dihydrogenphosphides of Alkali Metals, MPH2 (M ≙ Li, Na, K, Rb, Cs)The dihydrogenphosphides from lithium to cesium were obtained by the reaction of PH3 with the corresponding solutions of the metals or the metal amides in ammonia. The compounds were examined by X-ray, IR-spectroscopic, and thermochemical techniques.LiPH2 is not stable at room temperature, while evolving PH3 it decomposes to yellow products. NaPH2 is a stable, white compound; above 393 K it decomposes associated with discolouring. KPH2 and RbPH2 exist in the region from 110 K to ∼400 K in three crystalline forms. Its high-temperature modification is of the sodium chloride-type structure; a monoclinic deformation occurs with decreasing temperature. DSC-measurements revealed a further low temperature form.CsPH2 crystallizes in the CsCl-type structure between 110 K and ∼400 K.
    Notes: Die Dihydrogenphosphide von Lithium bis Caesium wurden durch Umsetzung der Lösungen der Alkalimetalle bzw. der Alkalimetallamide in Ammoniak mit überschüssigem Phosphin dargestellt. Röntgenographische, IR-spektroskopische und thermochemische Untersuchungen an den Verbindungen wurden durchgeführt.LiPH2 ist bei Raumtemperatur instabil und geht unter PH3-Abgabe in gelbe Zersetzungsprodukte über. NaPH2 ist eine stabile, weiße Verbindung, die sich unter Verfärbung oberhalb 393 K zersetzt.Vom KPH2 und RbPH2 existieren jeweils drei kristalline Phasen im Bereich von 110 K bis etwa 400 K. Die Hochtemperaturform kristallisiert im NaCl-Strukturtyp; mit sinkender Temperatur tritt eine monokline Verzerrung ein. Die Tieftemperaturform konnte nur über DSC-Messungen nachgewiesen werden. Für CsPH2 liegt im Bereich von 110 K bis etwa 400 K der CsCl-Strukturtyp vor.
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