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1.
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
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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
4.
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
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The synthesis of two formyl 2‐tetrazenes, namely, (E)‐1‐formyl‐1,4,4‐trimethyl‐2‐tetrazene ( 2 ) and (E)‐1,4‐diformyl‐1,4‐dimethyl‐2‐tetrazene ( 3 ), by oxidation of (E)‐1,1,4,4‐tetramethyl‐2‐tetrazene ( 1 ) using potassium permanganate in acetone solution is presented. Compound 3 was also synthesized in an improved yield from the oxidation of 1‐formyl‐1‐methylhydrazine ( 4a ) using potassium permanganate in acetone. Both compounds 2 and 3 were characterized by analytical (elemental analysis, GC‐MS) and spectroscopic methods (1H, 13C, and 15N NMR spectroscopy, and IR and Raman spectroscopy). In addition, the solid‐state structures of the compounds were confirmed by low‐temperature X‐ray analysis. (Compound 2 : triclinic; space group P‐1; a=5.997(1) Å, b=8.714(1) Å, c=13.830(2) Å; α=107.35(1)°, β=90.53(1)°, γ=103.33(1)°; VUC=668.9(2) Å3; Z=4; ρcalc=1.292 cm?3. Compound 3 : monoclinic; space group P21/c; a=5.840(2) Å, b=7.414(3) Å, c=8.061(2) Å; β=100.75(3)°; VUC=342(2) Å3; Z=2; ρcalc=1.396 g cm?3.) The vibrational frequencies of compounds 2 and 3 were calculated using the B3LYP method with a 6‐311+G(d,p) basis set. We also computed the natural bond orbital (NBO) charges using the rMP2/aug‐cc‐pVDZ method and the heats of formation were determined on the basis of their electronic energies. Furthermore, the thermal stabilities of these compounds, as well as their sensitivity towards classical stimuli, were also assessed by differential scanning calorimetry and standard BAM tests, respectively. Lastly, the attempted synthesis of (E)‐1,2,3,4‐tetraformyl‐2‐tetrazene ( 6 ) is also discussed. 相似文献
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In this contribution the synthesis and full structural as well as spectroscopic characterization of three 5‐(1,2,4‐triazol‐3‐yl)tetrazoles along with selected energetic moieties like nitro, nitrimino, and azido groups are presented. The main goal is a comparative study on the influence of those variable energetic moieties on structural and energetic properties. A complete characterization including IR and Raman as well as multinuclear NMR spectroscopy of all compounds is presented. Additionally, X‐ray crystallographic measurements were performed and reveal insights into structural characteristics as well as inter‐ and intramolecular interactions. The standard enthalpies of formation were calculated for all compounds at the CBS‐4M level of theory and reveal high positive heats of formation for all compounds. The calculated detonation parameters (using the EXPLO5.05 program) are in the range of 8000 m s?1 (8097 m s?1 ( 5 ), 8020 m s?1 ( 6 ), 7874 m s?1 ( 7 )). As expected, the measured impact and friction sensitivities as well as decomposition temperatures strongly depend on the energetic moiety at the triazole ring. The C? C connection of a triazole ring with its opportunity to introduce a large variety of energetic moieties and a tetrazole ring, implying a large energy content, leads to the selective synthesis of primary and secondary explosives. 相似文献
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Andreas Nordheider Tristram Chivers Oliver Schön Konstantin Karaghiosoff Kasun S. Athukorala Arachchige Alexandra M. Z. Slawin Prof. Dr. J. Derek Woollins 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(3):704-712
A new structural arrangement Te3(RPIII)3 and the first crystal structures of organophosphorus(III)–tellurium heterocycles are presented. The heterocycles can be stabilized and structurally characterized by the appropriate choice of substituents in Tem(PIIIR)n (m=1: n=2, R=OMes* (Mes*=supermesityl or 2,4,6‐tri‐tert‐butylphenyl); n=3, R=adamantyl (Ad); n=4, R=ferrocene (Fc); m=n=3: R=trityl (Trt), Mesor by the installation of a PV2N2 anchor in RPIII[TePV(tBuN)(μ‐NtBu)]2 (R=Ad, tBu). 相似文献
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Sophia J. Makowski Daniel Gunzelmann Jürgen Senker Wolfgang Schnick Prof. Dr 《无机化学与普通化学杂志》2009,635(15):2434-2439
Calcium hydrogenmelonate heptahydrate Ca[HC6N7(NCN)3] · 7H2O was obtained by metathesis reaction in aqueous solution. The structure of the molecular salt was elucidated by single‐crystal X‐ray diffraction. The crystal structure consists of alternating layers of planar monopronated melonate ions, Ca2+ and crystal water molecules. The anions of adjacent layers are staggered so that no π–π stacking occurs. The melonate entities are interconnected by hydrogen bonds within and between the layers. Ca[HC6N7(NCN)3] · 7H2O was investigated by solid‐state NMR and FTIR spectroscopy, TG and DTA measurements. 相似文献
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Alexander A. Dippold Prof. Dr. Thomas M. Klapötke 《Chemistry (Weinheim an der Bergstrasse, Germany)》2012,18(52):16742-16753
In this contribution, the synthesis and full structural and spectroscopic characterization of five bis‐1,2,4‐triazoles in combination with different energetic moieties like amino, nitro, nitrimino, azido, and dinitromethylene groups is presented. The main goal is a comparative study on the influence of those energetic moieties on the structural and energetic properties. A complete characterization including IR, Raman, and multinuclear NMR spectroscopy of all compounds is presented. Additionally, X‐ray crystallographic measurements were performed and deliver insight into structural characteristics as well as inter‐ and intramolecular interactions. The standard enthalpies of formation were calculated for all compounds at the CBS‐4M level of theory, the detonation parameters were calculated by using the EXPLO5.05 program. Additionally, the impact as well as the friction sensitivities and the sensitivity against electrostatic discharge were determined. The potential application of the synthesized compounds as energetic material will be studied and evaluated by using the experimentally obtained values for the thermal decomposition, the sensitivity data, and the calculated performance characteristics. 相似文献
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Jun‐Jie Wang Dao‐Jun Zhang Ren‐Chun Zhang Huan‐Huan Jin Xiao‐Fang Gao 《无机化学与普通化学杂志》2014,640(2):497-503
Two new co‐crystals based on 1,2,4,5‐benzenetetracarboxylic acid, (H2BETC)(H4tpim)](NO3) ( 1 ) and [(H4BETC)0.5(H2BETC)0.5(HVB4)](H2O) ( 2 ) [H4BETC = 1,2,4,5‐benzenetetracarboxylic acid, Htpim = 2,4,5‐tri(4‐pyridyl)‐imidazole, and VB4 = adenine], were synthesized and characterized by elemental analyses, IR spectroscopy, single‐crystal X‐ray diffraction, and X‐ray powder diffraction analysis. Compounds 1 and 2 were further assembled to form 3D supramolecular frameworks with 1D channels by intermolecular C–H ··· O, O–H ··· O, and N–H ··· O hydrogen‐bonding interactions. The results reveal that the structural differences of 1 and 2 may be attributed to different molecular components. Moreover, the UV/Vis and luminescent spectra of ligands and corresponding compounds were briefly investigated. 相似文献
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Dr. Niko Fischer Dániel Izsák Prof. Dr. Thomas M. Klapötke Dr. Jörg Stierstorfer 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(27):8948-8957
5‐(Tetrazol‐1‐yl)‐2H‐tetrazole ( 1 ), or 1,5′‐bistetrazole, was synthesized by the cyclization of 5‐amino‐1H‐tetrazole, sodium azide and triethyl orthoformate in glacial acetic acid. A derivative of 1 , 2‐methyl‐5‐(tetrazol‐1‐yl)tetrazole ( 2 ) can be obtained by this method starting from 5‐amino‐2‐methyl‐tetrazole. Furthermore, selected salts of 1 with nitrogen‐rich and metal (alkali and transition metal) cations, including hydroxylammonium ( 4 ), triaminoguanidinium ( 5 ), copper(I) ( 8 ) and silver ( 9 ), as well as copper(II) complexes of both 1 and 2 were prepared. An intensive characterization of the compounds is given, including vibrational (IR, Raman) and multinuclear NMR spectroscopy, mass spectrometry, DSC and single‐crystal X‐ray diffraction. Their sensitivities towards physical stimuli (impact, friction, electrostatic) were determined according to Bundesamt für Materialforschung (BAM) standard methods. Energetic performance (detonation velocity, pressure, etc.) parameters were calculated with the EXPLO5 program, based on predicted heats of formation derived from enthalpies computed at the CBS‐4M level of theory and utilizing the atomization energy method. From the analytical and calculated data, their potential as energetic materials in different applications was evaluated and discussed. 相似文献
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Jin‐Peng Geng Prof. Dr. Zhao‐Xi Wang Qiong‐Fang Wu Ming‐Xing Li Prof. Dr. Hong‐Ping Xiao 《无机化学与普通化学杂志》2011,637(2):301-305
A new manganese(II) complex [Mn3(bidc)2(C2O4)(H2O)10]n ( 1 ) (bidc = benzimidazole‐5,6‐dicarboxylate) was synthesized and characterized by X‐ray crystallography. X‐ray diffraction shows that complex 1 has a neutral, one‐dimensional (1D) brick wall chain structure. With the intramolecular and intermolecular hydrogen bonding interactions, the adjacent chains are joined into a 3D suparmolecular architecture. IR spectroscopy and variable temperature magnetic susceptibility measurements were made, which indicated weak antiferromagnetic coupling between the MnII ions in complex 1 . 相似文献
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Prof. Aleksei B. Sheremetev Nataly S. Aleksandrova Nadezhda V. Palysaeva Marina I. Struchkova Vladimir A. Tartakovsky Kyrill Yu. Suponitsky 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(37):12446-12457
An efficient two‐step one‐pot protocol for the synthesis of N‐nitrated trinitroethylamino furazans in an ionic liquid has been developed involving the condensation of aminofurazans with trinitroethanol and the N‐nitration of an intermediate Mannich base. Trinitroethylnitramino derivatives have been synthesized and characterized by multinuclear NMR spectroscopy and X‐ray crystallography. A role of the N,2,2,2‐tetranitroethylamino group for stabilization of the high‐density crystal‐packing motif is described. The performance calculations gave detonation pressures and velocities for the furazan derivatives in a range of about 31–36 GPa and 8330–8745 ms?1, respectively, which makes them competitive energetic materials. Furthermore, due to the positive oxygen balance, the compounds could be potential oxidizers for energetic formulations. 相似文献
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Michael Veith Prof. Dr. Dr. h.c. Andreas Rammo Oliver Schütt Volker Huch 《无机化学与普通化学杂志》2010,636(7):1212-1221
The branched tripodal chloro‐methyl‐siloxanes of the general formula tBuSi[{OSiMe2}yOSiMe3–xClx]3 [x = 0–3; y = 0–2] were synthesized, starting with tert‐Butyl‐trisilanol ( 1 ). The treatment of 1 with the chloro‐methyl‐silanes (Me3–xSiClx+1) (x = 0–3) in the presence of triethylamine leads to the compounds tBuSi(OSiMe2Cl)3 ( 2 ), tBuSi(OSiMeCl2)3 ( 3 ) and tBuSi(OSiCl3)3 ( 4 ). The siloxanes 2 – 4 are colourless oily liquids, which can be purified by distillation. Their yields decrease with the number of chloro substituents. In the reaction of compound 2 with three equivalents of water the silantriol tBuSi(OSiMe2OH)3 ( 5 ) is generated which is used to create the branched tripodal chloro‐methyl‐siloxanes tBuSi(OSiMe2OSiMe3)3 ( 6 ), tBuSi(OSiMe2OSiMe2Cl)3 ( 7 ), tBuSi(OSiMe2OSiMeCl2)3 ( 9 ) and tBuSi(OSiMe2OSiCl3)3 ( 10 ). Compound ( 7 ) is only a side product with a yield of 25 %., The cyclic tBuSi[{(OSiMe2)2Cl}(OSiMe2)3O] ( 8 ) can be isolated and characterised. The transformation of the compound tBuSi(OSiMe2OSiMe2Cl)3 ( 7 ) into the trisilanol tBuSi(OSiMe2OSiMe2OH)3 ( 11 ) allows to prepare the tripodale siloxane tBuSi(OSiMe2OSiMe2OSiMe3)3 ( 12 ) in good yields., The reaction of tBuSi(OSiMe2Cl)3 ( 2 ) with tert‐butyl trisilanol 1 leads to the formation of bicyclic tBuSi(OSiMe2O)3SitBu ( 13 ). An X‐ray structure determination on 13 reveals a [3.3.3]‐bicycle with a C3 axis, which crystallizes in the cubic crystal system in the space group Pa . The reported compounds 2 – 13 were characterised by NMR‐ and IR spectroscopy ( 5 , 11 ) and show correct elemental analyses. The 29Si‐NMR‐data of the compounds show interesting trends with respect to the Si–O chain length and the chloro substistuents. 相似文献
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The 2‐tert‐butyl, 2‐phenoxy, and 2‐diethylamino derivatives of 1,3‐bis(trimethylsilyl)‐1,3,2‐diazaphospha‐[3]ferrocenophane were prepared, and the molecular structure of the latter was determined by X‐ray diffraction. The phosphines could be oxidized by their slow reactions with sulfur or selenium, and the molecular structures of three sulfides and one selenide were determined. In contrast, the synthesis of oxides was less straightforward. All new compounds were characterized in solution by multinuclear magnetic resonance methods (1D and 2D 1H, 13C, 15N, 29Si, 31P, and 77Se NMR spectroscopy). 相似文献
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Maxim N. Sokolov Pavel A. Abramov Maxim A. Mikhailov Eugenia V. Peresypkina Alexander V. Virovets Vladimir P. Fedin 《无机化学与普通化学杂志》2010,636(8):1543-1548
Direct reaction of stoichiometric amounts of KBr, tantalum and bromine at 720 °C, followed by extraction and crystallization gives Ta6Br14 · 7H2O (1) . This compound slowly aquates into [(Ta6Br12)(H2O)6]2+, which crystallized as mixed Cs+/Br– ( 2 ), Cl– ( 3 ) and SO42– ( 4 ) salts. In Bu4NBr melt, 1 undergoes oxidation into (Bu4N)2[(Ta6Br12)Br6] ( 5 ). Reaction of 1 with dimethylsulfoxide also induces oxidation of the { Ta6Br12} 2+ core into { Ta6Br12} 4+, and the corresponding complex [(Ta6Br12)(dmso)2Cl4] · iPrOH · 4.8H2O ( 6 ) was isolated and structurally characterized. Molecular and crystal structures for 2 – 6 were determined. 相似文献
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Günter Motz Thomas Schmalz Germund Glatz Rhett Kempe Wolfgang Milius Bernd Wrackmeyer Prof. Dr. 《无机化学与普通化学杂志》2010,636(6):1056-1060
Ammonolysis of 1,2‐bis[dichloro(methyl)silyl]ethane afforded a crystalline tricyclic silazane along with polymeric material. The crystalline material could be isolated in pure state. It was analyzed by 1H, 13C, 15N and 29Si NMR spectroscopy in solution, by 13C, 15N and 29Si MAS NMR spectroscopy in the solid state, as well as by single‐crystal and powder X‐ray diffraction. The title compound exists as a single isomer in solution, whereas in the solid state the presence of several modifications is indicated, in particular by the solid‐state MAS NMR spectra. 相似文献
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From Amino Acids to High‐Energy Dense Oxidizers: Polynitro Materials Derived from β‐Alanine and L‐Aspartic Acid 下载免费PDF全文
New oxygen‐rich compounds starting from the amino acids β‐alanine and L ‐aspartic acid were synthesized and comprehensively analyzed including multinuclear NMR spectroscopy and vibrational spectroscopy. Thermal stabilities were measured and the behavior towards external stimuli like friction or impact were determined. Detonation and combustion parameters were predicted by using the EXPLO5 V6.02 code and were compared with common explosives. In addition, crystal structures were obtained for two compounds. 相似文献
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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