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Friedrich-Wilhelm-Lübke-Koog, Germany

Deblitz R.,Nammo Germany GmbH | Hrib C.G.,Otto Von Guericke University of Magdeburg | Plenikowski G.,Nammo Germany GmbH | Edelmann F.T.,Otto Von Guericke University of Magdeburg
Crystals | Year: 2012

The title compound [H2NNHC(NH2)2]2[C6HO2(NO2)3] (2) was prepared in 85% yield by treatment of sodium styphnate with 2 equivalents of aminoguanidinium nitrate, followed by crystallization from aqueous solution. Compound 2 crystallizes in the triclinic space group Pī with unit cell dimensions a = 6.7224(3) Å, b = 10.7473(4) Å, c = 11.9604(5) Å, α = 113.212(4)°, β = 90.579(3)°, γ = 99.815(3)°, V = 779.68(6) Å3, Z = 2. In the solid state structure of 2, no water of crystallization is present. Bond angles within the aromatic ring of the styphnate anion indicate a significant distortion with larger angles (122.04(18)-125.96(18) Å) at the carbons bearing the nitro groups, and smaller ones (113.30(17) and 114.07(17) Å) at the C-O- carbon atoms. The crystal structure of 2 consists of layers formed by an extensive network of N-H⋯O hydrogen bonds between NH2 groups of the aminoguanidinium cation and the negatively charged oxygens of the styphnate anion. The layers are again interconnected by N-H⋯N hydrogen bonds between neighboring aminoguanidinium cations. © 2011 by the authors; licensee MDPI, Basel, Switzerland.

Deblitz R.,Nammo Germany GmbH | Hrib C.G.,Otto Von Guericke University of Magdeburg | Plenikowski G.,Nammo Germany GmbH | Edelmann F.T.,Otto Von Guericke University of Magdeburg
Inorganic Chemistry Communications | Year: 2012

The first metal-organic azotetrazolate, [Me 3Sn(μ-C 2N 10)SnMe 3(H 2O)] n (2), was prepared in 61% isolated yield by the reaction of disodium azotetrazolate (Na 2AZT· 5H 2O, 1) with 2 equivalents of Me 3SnCl in aqueous solution. An X-ray diffraction study revealed a novel supramolecular structure of 2 in the crystal. Two different coordination environments around tin result in the formation of an unexpected zig-zag chain structure in the solid state with H 2O ligands coordinated to every second Sn atom ligands terminating the alternating corners of the zig-zag chain. Both hydrogen atoms of the coordinated water molecules are engaged in O-H⋯N to different azotetrazolate dianions, leading to an interlocking of the zig-zag chain in a zipper-like overall crystal structure. Despite its fairly low nitrogen content of only 27.48% the title compound was found to be sensitive to both impact and friction. © 2012 Elsevier B.V. All rights reserved.

Deblitz R.,Otto Von Guericke University of Magdeburg | Hrib C.G.,Otto Von Guericke University of Magdeburg | Blaurock S.,Otto Von Guericke University of Magdeburg | Jones P.G.,TU Braunschweig | And 2 more authors.
Inorganic Chemistry Frontiers | Year: 2014

A series of potentially explosive Werner-type cobalt(iii) complexes comprising the anions azotetrazolate, nitrotetrazolate, picrate and dipicrylamide were prepared via simple metathetical routes. Treatment of [Co(NH3)5NO2]Cl2, trans-[Co(NH3)4(py)NO2]Cl2 (py = pyridine), trans-[Co(NH3)4(NO2)2]Cl, and [Co(NH3)5N3]Cl2 with equimolar amounts of disodium azotetrazolate, (Na2C2N10·5H2O, 1), in aqueous solutions afforded new cobalt(iii) azotetrazolate salts [Co(NH3)5NO2](C2N10)·2H2O (2), trans-[Co(NH3)4(py)NO2](C2N10)·2H2O (3), trans-[Co(NH3)4(NO2)2]2(C2N10) (4), and [Co(NH3)5N3](C2N10)·H2O (5) in moderate to excellent yields (46-88%). Similar treatment of trans-[Co(NH3)4(NO2)2]Cl with 1 equiv. of sodium 5-nitrotetrazolate dihydrate (= NaNT, 6) afforded the novel cobalt(iii) 5-nitrotetrazolate derivative trans-[Co(NH3)4(NO2)2](NT)·H2O (7) as orange, rectangular prismatic crystals in 64% yield. Two complex cobalt(iii) picrates, trans-[Co(NH3)4(NO2)2](picrate)·H2O (9) and [Co(NH3)5N3](picrate)2 (10), were prepared in a similar manner from the corresponding chloride precursors and equimolar amounts of sodium picrate. The reaction of trans-[Co(NH3)4(NO2)2]Cl with sodium dipicrylamide (= NaDPA) in a 1 : 1 molar ratio gave the first cobalt(iii) dipicrylamide, trans-[Co(NH3)4(NO2)2](DPA)·H2O (12). Finally, the highly explosive, dark blue-green dichroitic non-electrolyte complex mer-[Co(en)(py)(N3)3] (13) was formed upon treatment of [Co(en)(py)2(NH3)Cl]Cl2·H2O with excess NaN3 in hot water (93% yield). The molecular and crystal structures of 2, 3, 4, 5, 7, 9, 10, 12, and 13 were determined by single-crystal X-ray diffraction. In the solid state, all compounds comprised extensive hydrogen-bonded supramolecular networks. Representative studies of the energetic properties (impact and friction sensitivity, combustion) revealed that some of the new compounds can be classified as primary explosives. This journal is © the Partner Organisations 2014.

Stock G.,Otto Von Guericke University of Magdeburg | Hrib C.G.,Otto Von Guericke University of Magdeburg | Deblitz R.,Nammo Germany GmbH | Kuhling M.,Otto Von Guericke University of Magdeburg | And 2 more authors.
Inorganic Chemistry Communications | Year: 2014

The first metal-organic 5-nitrotetrazolate, [Me3Sn(μ-OH) SnMe3(μ-OH)SnMe3(H2O)][NT] (2), has been prepared by a simple metathetical reaction between Me3SnCl and sodium 5-nitrotetrazolate dihydrate (= NaNT, 1). A single-crystal X-ray diffraction study revealed the presence of the trinuclear [Me3Sn(μ-OH) SnMe3(μ-OH)SnMe3(H2O)]+ cation to which the 5-nitrotetrazolate anion is coordinated via a ring-N atom. The NT anion is further engaged in four different OHâ̄N and OHâ̄N hydrogen bonds involving the remaining three ring-nitrogen atoms and one oxygen of the nitro group, leading to an extensive supramolecular hydrogen-bonded network in the solid state. Despite its very low N content of only 10.65%, compound 2 is highly impact-sensitive (< 2.5 J) and can be classified as a primary explosive. © 2014 Elsevier B.V.

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