Notizen: Zur Kenntnis eines Siliciumtetrazids Si(N<sub>3</sub>)<sub>4</sub>

Wiberg, Egon; Michaud, Horst

doi:10.1515/znb-1954-0717

Cited by 12 publications

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“…In comparison, structural information for analogous silicon compounds is lacking. Thus far, only Si(N 3 ) 4 has been reported to be a violently explosive substance, 6 which was prepared in situ and characterized by 29 Si NMR or IR spectroscopy. 7 Following our interest in main-group element azides with a high nitrogen content, 8 we describe here the synthesis and full characterization of the [Si(N 3 ) 6 ] 2-ion.…”

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confidence: 99%

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The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular Structure

2002

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The reaction of SiCl4 with an excess of (PPN)N3 (PPN+ = [(Ph3P)2N]+) affords selectively (PPN)2[Si(N3)6] (1). Simultaneous thermal analysis (TG-DTA) shows that the hexaazidosilicate salt is remarkably stable, melting at Tonex = 214 degrees C. Melting of 1 is followed by two distinct exothermic decomposition processes at Ton = 256 and 321 degrees C, the first one involving elimination of N2 and the second one degradation of the PPN cations and evolution of Si(N3)4, N2, and some HN3. The crystal structure of 1 consists of discrete PPN+ cations and S2 symmetric [Si(N3)6]2- anions, which have a very rare, octahedral SiN6 framework and the highest nitrogen content (90%) among the hexaazidometallates reported so far. The IR, Raman, 29Si, and 14N NMR spectra of 1 in CH3CN suggest in combination with the calculated spectra the presence of intact [Si(N3)6]2--anions of S6 symmetry in solution. Geometry optimizations with various methods and basis sets show an S6 symmetric structure to be the most stable [Si(N3)6]2- isomer, the calculated bonding parameters comparing well with the experimental values.

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confidence: 99%

“…Treatment of a solution of SiCl 4 in CH 3 CN with an excess of (PPN)N 3 at 0°C leads selectively to (PPN) 2 [Si(N 3 ) 6 ] (1) as evidenced by IR monitoring of the reaction (equation).…”

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confidence: 99%

The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular Structure

2002

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“…All of these observations imply that 1 is of limited use as a starting material for the preparation of Lewis base adducts of Si(N 3 ) 4 . Therefore, the synthesis of Si(N 3 ) 4 was attempted and for this purpose the reaction of SiCl 4 with excess NaN 3 in refluxing benzene was reinvestigated 9a. 23 Monitoring of the reaction progress by 14 N NMR spectroscopy revealed a slow conversion in the absence of an azido group transfer catalyst, which led to an equilibrium mixture containing three products in the approximate ratio 1.8:2.9:1 13.…”

Section: Methodsmentioning

confidence: 99%

Neutral Lewis Base Adducts of Silicon Tetraazide

et al. 2010

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Highly energetic and still stable: The first base adducts of silicon tetraazide, Si(N3)4(L2) (L2=bipyridine, 1,10‐phenanthroline), were prepared and fully characterized (picture: the ball and stick model of the adduct with L2=2,2'‐bipyridine in front of its FTIR spectrum; dark gray C, white H, light gray Si, blue N). The highly energetic compounds combine a remarkable thermal stability, with a high reactive nitrogen content (up to 48 %) and convenient accessibility.

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“…29,[41][42][43] The experimental investigation [50][51][52] of N-rich tetrazolato complexes poses primarily two challenges: the potential for high energy density, percussion sensitivity and thermal lability and the fact that most pblock element-tetrazole compounds are prone to hydrolysis. [53][54][55][56] In this paper we describe a convenient synthetic route to poly(tetrazolato) complexes based on the intriguing four reactive centres of the previously described N-rich, highly endothermic tetraazides of the type Si(N 3 ) 4 (L 2 ), 53 L 2 = 2,2'-bipyridine (bpy), 1,10-phenanthroline (phen); 51,52,57,58 see ref.…”

Section: -Substituted Tetrazole Derivatives With the Exception Of Mementioning

confidence: 99%

Synthesis of six-coordinate mono-, bis-, and tris(tetrazolato) complexes via [3 + 2] cycloadditions of nitriles to silicon-bound azido ligands

Portius

Davis

2016

Dalton Trans.

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Article:Portius, P. orcid.org/0000-0001-8133-8860 and Davis, M. (2016) ReuseUnless indicated otherwise, fulltext items are protected by copyright with all rights reserved. The copyright exception in section 29 of the Copyright, Designs and Patents Act 1988 allows the making of a single copy solely for the purpose of non-commercial research or private study within the limits of fair dealing. The publisher or other rights-holder may allow further reproduction and re-use of this version -refer to the White Rose Research Online record for this item. Where records identify the publisher as the copyright holder, users can verify any specific terms of use on the publisher's website. TakedownIf you consider content in White Rose Research Online to be in breach of UK law, please notify us by emailing eprints@whiterose.ac.uk including the URL of the record and the reason for the withdrawal request. Abstract. A convenient synthetic route to poly(tetrazolato) silicon complexes is described based on the four reactive centres of the N-rich, highly endothermic tetraazides of the type Si(N 3 ) 4 (L 2 ). Hypercoordinate azido(tetrazolato) silicon complexes Si(N 3 ) 2 (N 4 C-R) 2 (L 2 ), R = CH 3 , C 6 H 5 , 4-C 6 H 4 CH 3 (4a, 5, 6, 7) and Si(N 3 ) 2 (N 4 C-L) 2 (9, L = 2-C 5 H 4 N), L 2 = 2,2'-bipyridine, 1,10-phenanthroline, with SiN 6 skeletons were synthesised via multiple [3+2] dipolar cycloaddition reactions starting from Si(N 3 ) 4 (L 2 ) and a nitrile. The isolated new complexes were characterised by standard analytical methods, single crystal Xray diffraction and Differential scanning calorimetry (4a,b). Tetrazolato ligand linkage isomerism was observed for complex 4a. The crystallographically characterised methyl tetrazolato complexes and plausible configurational and linkage isomers were evaluated by DFT calculations on the B3LYP/6-311G(d,p) level. CREATED USING THE RSC ARTICLE TEMPLATE (VER. 3.1) -SEE WWW.RSC.ORG/ELECTRONICFILES FOR DETAILS

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Notizen: Zur Kenntnis eines Siliciumtetrazids Si(N₃)₄

Cited by 12 publications

References 0 publications

The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular Structure

The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular Structure

Neutral Lewis Base Adducts of Silicon Tetraazide

Synthesis of six-coordinate mono-, bis-, and tris(tetrazolato) complexes via [3 + 2] cycloadditions of nitriles to silicon-bound azido ligands

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Notizen: Zur Kenntnis eines Siliciumtetrazids Si(N3)4

Cited by 12 publications

References 0 publications

The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular Structure

The Hexaazidosilicate(IV) Ion: Synthesis, Properties, and Molecular Structure

Neutral Lewis Base Adducts of Silicon Tetraazide

Synthesis of six-coordinate mono-, bis-, and tris(tetrazolato) complexes via [3 + 2] cycloadditions of nitriles to silicon-bound azido ligands

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Notizen: Zur Kenntnis eines Siliciumtetrazids Si(N₃)₄