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1.
Niko Fischer Prof. Dr. Thomas M. Klapötke Davin G. Piercey Jörg Stierstorfer 《无机化学与普通化学杂志》2012,638(2):302-310
The hydroxylammonium salts of monodeprotonated 5‐nitriminotetrazole ( 4 ), double deprotonated 5‐nitriminotetrazole ( 5 ), 1‐methyl‐5‐nitriminotetrazole ( 6 ), and 2‐methyl‐5‐nitraminotetrazole ( 7 ) have been prepared in high yield from the corresponding 5‐nitriminotetrazoles as free acids and an aqueous solution of hydroxylamine or the metathesis reactions of hydroxylammonium hydrochloride with the silver salt of the corresponding nitriminotetrazole, respectively. The energetic salts 4 – 7 were fully characterized by single‐crystal X‐ray diffraction ( 4 – 6 ), NMR spectroscopy, IR‐ and Raman spectroscopy as well as DSC measurements. The sensitivities towards impact, friction and electrical discharge were determined. In addition, several detonation parameters (e.g. heat of explosion, detonation velocity) were computed by the EXPLO5.04 computer code based on calculated (CBS‐4M) heats of formation and X‐ray densities. 相似文献
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3.
Thomas M. Klaptke Jrg Stierstorfer Karina R. Tarantik Ines D. Thoma 《无机化学与普通化学杂志》2008,634(15):2777-2784
The new compounds strontium 5‐nitriminotetrazolate dihydrate ( 1 ), strontium bis(1‐hydro‐5‐nitriminotetrazolate) tetrahydrate ( 2 ), strontium bis(1‐methyl‐5‐nitriminotetrazolate) monohydrate ( 3 ) and strontium bis(2‐methyl‐5‐nitraminotetrazolate)·x H2O (x = 2–4) ( 4 ) were synthesized by the reactions of strontium hydroxide octahydrate and 5‐nitriminotetrazole ( 5 ), 1‐methyl‐5‐nitriminotetrazole ( 6 ) and 2‐methyl‐5‐nitraminotetrazole ( 7 ), respectively. The compounds were characterized using multinuclear NMR spectroscopy, vibrational (IR and Raman) spectroscopy, elemental analysis and differential scanning calorimetry. The solid state structures of 1 , 2 , 3 and 4 were determined using low temperature X‐ray diffraction. In addition, the sensitivities (impact, friction, electrical discharge) of 1 – 4 were investigated and their use as red colorants in pyrotechnic compositions was tested. 相似文献
4.
The synthesis of the polynitroaromatic compound pentanitrobenzene was re‐examined by modern spectroscopic, structural and physicochemical methods. Originally prepared in 1979, this material could exhibit interesting properties as an oxygen‐rich energetic building block. The energies of formation were calculated with the GAUSSIAN program package and the detonation parameters were predicted using the EXPLO5 computer code. The performance data were determined and compared to the common oxidizer ammonium perchlorate. The crystal structure of pentanitrobenzene was determined by X‐ray crystallography, and those of 2,3,4,6‐tetranitroaniline and styphnic acid (trinitroresorcinol) were re‐determined. 相似文献
5.
This study presents the preparation of 5‐azido‐3‐nitro‐1H‐1, 2,4‐triazole ( 1 ) in both good yield and high purity, starting from commercially available chemicals in a three step synthesis. Furthermore, several metal and nitrogen‐rich salts with sodium ( 3 ), potassium ( 4 ), cesium ( 5 ), silver ( 6 ), lead ( 7 ), ammonium ( 8 ), guanidinium ( 9 ), and aminoguanidinium ( 10 ) were prepared by simple acid‐base reactions. All compounds were well characterized by various means, including vibrational (IR, Raman) and multinuclear (1H, 13C, 14N, 15N) NMR spectroscopy, mass spectrometry, and DSC. Additionally the structure of 7 was determined by single‐crystal X‐ray diffraction. The sensitivities towards various outer stimuli (impact, friction, electrostatic discharge) were determined according to BAM standards. The metal salts were tested as potential primary explosives utilizing various preliminary tests. 相似文献
6.
The synthesis of 3,3′‐bis(dinitromethyl)‐5,5′‐azo‐1H‐1,2,4‐triazole ( 5 ) using the readily available starting material 2‐(5‐amino‐1H‐1,2,4‐triazol‐3‐yl)acetic acid ( 1 ) is described. All compounds were characterized by means of NMR, IR, and Raman spectroscopy. The energetic compound 5 was additionally characterized by single‐crystal X‐ray diffraction and DSC measurements. The sensitivities towards impact, friction and electrical discharge were determined. In addition, detonation parameters (e.g. heat of explosion, detonation velocity) of the target compound were computed using the EXPLO5 code based on the calculated (CBS‐4M) heat of formation and X‐ray density. 相似文献
7.
Dr. Marek Daszkiewicz Mariusz K. Marchewka Iryna Typilo Lubomir D. Gulay Dariya Semenyshyn 《无机化学与普通化学杂志》2011,637(10):1409-1413
The crystal structure of distrontium octacyanotungstate decahydrate, Sr2[W(CN)8] · 10H2O, was solved using X‐ray single crystal diffraction. The tungsten atom lies on a two fold axis. Eight cyanide anions create tetragonal antiprismatic coordination sphere of tungsten atom. The two edge‐sharing tetragonal antiprisms of [Sr(NC)3(OH2)5], create a dimer, [Sr2(CN)6(H2O)6(μ‐H2O)2], which lies on the inversion center. One symmetry independent water molecule is located in a void of 40 Å3. Vibrational (FT‐IR and FT‐Raman spectroscopic) behavior of main structural units is discussed. It was spectroscopically confirmed that the geometry of [W(CN)8]4– anion is slightly distorted from that corresponding to “free” anion. The number of observed bands is significantly lower than that expected for C2 point group. 相似文献
8.
This study features the preparation of three new energetic C‐azido‐1, 2, 4‐triazoles, with the anion of one being a new binary C–N compound. 5‐Azido‐1H‐1, 2, 4‐triazole‐3‐carbonitrile ( 1 ) was prepared from 5‐amino‐1H‐1, 2, 4‐triazole‐3‐carbonitrile and further derivatized to 5‐azido‐1H‐1, 2, 4‐triazole‐3‐carbohydroximoyl chloride ( 5 ) with 3‐azido‐1H‐1, 2, 4‐triazole‐5‐carboxamidoxime ( 3 ) as an intermediate. The ability of 1 and 3 for salt formation was shown with the respective silver salts 2 and 4 . All compounds were well characterized by various means, including IR and multinuclear NMR spectroscopy, mass spectrometry, and DSC. The molecular structures of 1 , 3 , and 5 in the solid state were determined by single‐crystal X‐ray diffraction. The sensitivities towards various outer stimuli (impact, friction, electrostatic discharge) were determined according to BAM standards. The silver salts were additionally tested for their potential as primary explosives. 相似文献
9.
Synthesis,Crystal Structure,Thermal and Explosive Properties of [Cd(SCZ)3(H2O)](PA)2·3H2O (SCZ = Semicarbazide,PA = Picrate)
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Wen‐Chao Tong Rui Zhang Lin‐Jun Xue Rui Xu Li‐Nong Zhang Tong‐Lai Zhang Li Yang 《无机化学与普通化学杂志》2015,641(7):1225-1229
The heptacoordinate transition metal coordination compound [Cd(SCZ)3(H2O)](PA)2 · 3H2O ( 1 ) with the ligand semicarbazide (SCZ) and the counteranion picrate (PA) was synthesized and characterized by elemental analysis and FTIR spectroscopy. Single‐crystal X‐ray diffraction analysis revealed that 1 crystallizes in the monoclinic space group P21/c. The Cd2+ ion is heptacoordinated by three SCZ groups and a water molecule. SCZ presents typical bidentate coordination modes. The thermal decomposition mechanism of 1 was studied by differential scanning calorimetry (DSC), which revealed that complex 1 exhibits three small endothermic and two large exothermic processes. The non‐isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa‐Doyle's method, respectively. The heat of combustion was measured by oxygen bomb calorimetry. The enthalpy of formation, the critical temperature of thermal explosion, the entropy of activation (ΔS≠), the enthalpy of activation (ΔH≠), and the free energy of activation (ΔG≠) were also calculated. Sensitivity tests revealed that 1 is insensitive to mechanical stimuli. 相似文献
10.
A straightforward way for the preparation of the energetic 5‐aminotetrazolium and 1, 5‐diaminotetrazolium salts is reported. The energetic salts were readily synthesized by the reaction of 5‐aminotetrazolium nitrate or 1, 5‐diaminotetrazolium nitrate with ammonium 5‐nitroiminotetrazolate, ammonium 1‐methyl‐5‐nitroiminotetrazolate, bis(ammonium) ethylene bis(5‐nitroiminotetrazolate), and diammonium iminobis(5‐tetrazolate), respectively, in water under mild conditions. All products were recovered as highly crystalline materials in excellent yields and purities, and were fully characterized by IR spectroscopy, 1H and 13C NMR spectroscopy, DSC measurements as well as elemental analyses. 相似文献
11.
Formaggio F Baldini C Moretto V Crisma M Kaptein B Broxterman QB Toniolo C 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(8):2395-2404
Terminally protected homopeptides of tert-leucine, from the dimer to the hexamer, co-oligopeptides of tert-leucine in combination with alpha-aminoisobutyric acid or glycine residues up to the hexamer level, and simple dipeptides representing known scaffolds for catalysts in asymmetric organic reactions were prepared by solution methods and fully characterized. The results of conformation analysis, performed by use of FT-IR absorption, NMR, CD, and X-ray diffraction techniques, indicate that this hydrophobic alpha-amino acid with tetrasubstitution at the Cbeta atom is structurally versatile. We show that it prefers extended or semiextended conformations, but can also be accommodated in folded structures, provided that these are biased by the presence of helicogenic residues. The current large-scale production of Tle, combined with its conformational preferences unravelled in this work, should make this bulky, hydrophobic, Calpha-trisubstituted alpha-amino acid a regular building block of any strategy seeking to tailor peptides with improved catalytic and pharmacological properties. 相似文献
12.
Two copper(I) complexes of compositions [Cu(HL)I]2 · EtOH ( 1 ) and [Cu(HL)3]I · MeOH ( 2 ) were synthesized via the reactions of HL [HL = 2(4,5‐diphenyl‐1H‐imidazol‐2‐yl)pyridine] and CuI in EtOH and MeOH, respectively, under solvothermal conditions. The complexes were characterized by X‐ray single crystal diffraction, IR spectroscopy, and elemental analysis. Compounds 1 and 2 are catalytically active towards ketalization reaction, giving various ketals under mild conditions. 相似文献
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Synthesis and Characterisation of Mercury Cyanamide HgCN2 was prepared by double conversion of HgCl2 with sodium cyanamide in aqueous solution. Its crystal structure has been determined using X‐ray powder data and refined by combined profile fits using X‐ray and neutron diffraction data (Pbca, Z = 8, a = 10.4851(1), b = 6.5138(1), c = 6.8929(1) Å; Rp (X‐ray) = 6.15%; Rp (neutrons) = 2.33; 2.43%). The cyanamide‐anion is bent (172.4(7)°), which has been confirmed by vibrational spectroscopy. Mercury and carbon form zigzag chains. Not including nitrogen, the structure is related to the MnP‐structure type. 相似文献
15.
Marta De Zotti Dr. Francesca Damato Fernando Formaggio Prof. Marco Crisma Dr. Elisabetta Schievano Dr. Stefano Mammi Prof. Bernard Kaptein Dr. Quirinus B. Broxterman Dr. Peter J. Felock Dr. Daria J. Hazuda Dr. Sheo B. Singh Dr. Jochen Kirschbaum Dr. Hans Brückner Prof. Claudio Toniolo Prof. 《Chemistry (Weinheim an der Bergstrasse, Germany)》2010,16(1):316-327
Integramide A is a 16‐amino acid peptide inhibitor of the enzyme HIV‐1 integrase. We have recently reported that the absolute stereochemistries of the dipeptide sequence near the C terminus are L ‐Iva14‐D ‐Iva15. Herein, we describe the syntheses of the natural compound and its D ‐Iva14‐L ‐Iva15 diastereomer, and the results of their chromatographic/mass spectrometric analyses. We present the conformational analysis of the two compounds and some of their synthetic intermediates of different main‐chain length in the crystal state (by X‐ray diffraction) and in solvents of different polarities (using circular dichroism, FTIR absorption, and 2D NMR techniques). These data shed light on the mechanism of inhibition of HIV‐1 integrase, which is an important target for anti‐HIV therapy. 相似文献
16.
Organotin compounds are a recurring motif in organometallic chemistry. The syntheses and characterization of new diorganotin compounds with α‐oxoglutaric acid isonicotinyl hydrazone are described, prepared compounds were characterized by elemental analysis, UV/Vis, 1H, and 13C NMR spectroscopy, and X‐ray diffraction. They both have a distorted pentagonal bipyramidal arrangement, with a heptacoordinated central tin atom. Compound 1 presents a centrosymmetric dinuclear framework. Interestingly, intermolecular O–H ··· N and O–H ··· O hydrogen bonds contribute to the two‐dimensional network. Compound 2 is a simple mononuclear compound, which exhibits a rare one‐dimensional chain constructed by intermolecular O–H ··· Cl and N–H ··· O hydrogen bonds. 相似文献
17.
Nitrogen‐Rich Alkali Metal Salts (Na and K) of [Bis(N,N‐bis(1H‐tetrazol‐5‐yl)amine)‐zinc(II)] Anion: Syntheses,Crystal Structures,and Energetic Properties
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Fugang Li Wenyuan Zhao Sitong Chen Tonglai Zhang Zunning Zhou Li Yang 《无机化学与普通化学杂志》2015,641(5):911-916
Two nitrogen‐rich alkali metal salts based on nitrogen‐rich anion [Zn(bta)2]2–: {[Na2Zn(bta)2(H2O)8] · H2O}n ( 1 ) and {[K2Zn(bta)2(H2O)4]}n ( 2 ) were synthesized by reactions of alkali hydroxide, N,N‐bis(1H‐tetrazol‐5‐yl)amine (H2bta), and zinc chloride in aqueous solutions. The crystal structures of 1 and 2 were determined by low temperature single‐crystal X‐ray diffraction and fully characterized by elemental analysis and FT‐IR spectroscopy. The structures demonstrate that an infinite 1‐dimensional (1D) chain structure is constructed by Na+ ions and bridging water molecules in compound 1 , which is connected by extensive hydrogen bonds forming a complex 3D network, whereas compound 2 features a more complicated 3D metal‐organic framework (MOF). The thermal behaviors of 1 and 2 were investigated by differential scanning calorimetry (DSC) measurements. The DSC results illustrate that both compounds exhibit high thermal stabilities (decomposition temperature > 345 °C). In addition, the heats of formation were calculated on the basis of the experimental constant‐volume energies of combustion measured by using bomb calorimetry. Lastly, the sensitivities towards impact and friction were assessed according to Bundesamt für Materialforschung (BAM) standard methods. 相似文献
18.
The nitration of 5‐amino‐1H‐tetrazole ( 1 ), 5‐amino‐1‐methyl‐1H‐tetrazole ( 3 ), and 5‐amino‐2‐methyl‐2H‐tetrazole ( 4 ) with HNO3 (100%) was undertaken, and the corresponding products 5‐(nitrimino)‐1H‐tetrazole ( 2 ), 1‐methyl‐5‐(nitrimino)‐1H‐tetrazole ( 5 ), and 2‐methyl‐5‐(nitramino)‐2H‐tetrazole ( 6 ) were characterized comprehensively using vibrational (IR and Raman) spectroscopy, multinuclear (1H, 13C, 14N, and 15N) NMR spectroscopy, mass spectrometry, and elemental analysis. The molecular structures in the crystalline state were determined by single‐crystal X‐ray diffraction. The thermodynamic properties and thermal behavior were investigated by using differential scanning calorimetry (DSC), and the heats of formation were determined by bomb calorimetric measurements. Compounds 2, 5 , and 6 were all found to be endothermic compounds. The thermal decompositions were investigated by gas‐phase IR spectroscopy as well as DSC experiments. The heats of explosion, the detonation pressures, and velocities were calculated with the software EXPLO5, whereby the calculated values are similar to those of common explosives such as TNT and RDX. In addition, the sensitivities were tested by BAM methods (drophammer and friction) and correlated to the calculated electrostatic potentials. The explosion performance of 5 was investigated by Koenen steel sleeve test, whereby a higher explosion power compared to RDX was reached. Finally, the long‐term stabilities at higher temperatures were tested by thermal safety calorimetry (FlexyTSC). X‐Ray crystallography of monoclinic 2 and 6 , and orthorhombic 5 was performed. 相似文献
19.
The reactions of 5‐nitriminotetrazole ( 4 ) with 1‐methyl‐5‐aminotetrazole ( 2 ) as well as 2‐methyl‐5‐aminotetrazole ( 3 ) were investigated. In the first reaction 2 was protonated yielding 1‐methyl‐5‐aminotetrazolium 5‐nitrimino‐1H‐tetrazolate monohydrate ( 7 ). In the latter case no protonation could be observed and a co‐crystallization of 5‐nitraminotetrazole and 2‐methyl‐5‐aminotetrazole was obtained. In this compound a new tautomer of 4 could be found. Both products were determined by low temperature single crystal X‐ray diffraction, IR, Raman and multinuclear (1H, 13C, 15N) NMR spectroscopy, elemental analysis as well as differential scanning calorimetry. In addition the heats of formation were calculated using experimentally obtained heats of combustion. With these and the X‐ray densities several detonation parameter were computed using the EXPLO5 software. In addition the sensitivities towards impact, friction and electrostatic discharge were determined. Further, two crystal structures of the important starting materials in energetic research 5‐nitriminotetrazole monohydrate ( 4 ·H2O) and 1‐methyl‐5‐nitriminotetrazolemonohydrate ( 5 ·H2O) are presented and compared with the water‐free compounds. The heats of formation of 4 , 4 ·H2O, 5 , 5 ·H2O have been calculated by the atomization method using the CBS basis set. Inclusion of crystal water decrease heats of formation about 265 kJ mol?1. Also the influence of crystal water on sensitivities (impact, friction, electrostatic discharge) but also performance is discussed. 相似文献
20.
Melamium salts are a group of ionic carbon nitride type compounds that has been investigated only scarcely. We herein present a novel representative of this group. A melamium thiocyanate melam (1:1) adduct was synthesized from dicyandiamide and ammonium thiocyanate in sealed glass ampoules. The structure of the adduct was determined from single‐crystal X‐ray diffraction. Melamium thiocyanate melam crystallizes in monoclinic space group P21/c (no. 14) with lattice parameters of a = 3.6041(11), b = 28.532(7), c = 10.937(4) Å, β = 99.051(14)°, and Z = 4. While the melamium ions form 2D extended hydrogen bridged networks, the thiocyanate ions are disordered and no distinct structural sites could be assigned to the respective atoms. Instead, continuous columns of electron density located in channels in the porous structure were identified as potential space for anion locations. The compound was further characterized by elemental analysis, FTIR spectroscopy and solid‐state MAS‐NMR spectroscopy of the nuclei 1H, 13C and 15N. Rietveld refinement of powder samples was performed for phase analysis. Furthermore, DSC‐TG was used to investigate the thermal behavior of the compound. 相似文献