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Journal of the American Chemical Society

Volumn 131, Issue 1, 2009, Pages 72-74

The binary silver nitrogen anion [Ag(N3)]2 -

(3) Klapötke, Thomas M a Krumm, Burkhard a Scherr, Matthias a

a UNIVERSITY OF MUNICH (Germany)

Author keywords

[No Author keywords available]

Indexed keywords

COORDINATION SPHERE; SILVER AZIDES;

COORDINATION REACTIONS; NEGATIVE IONS; NITROGEN COMPOUNDS;

SILVER;

ANION; AZIDE; EXPLOSIVE; NITROGEN DERIVATIVE; SILVER DERIVATIVE;

ARTICLE; CHEMICAL ANALYSIS; CHEMICAL STRUCTURE; CRYSTAL STRUCTURE; STRUCTURE ANALYSIS; SYNTHESIS;

EID: 67749142085 PISSN: 00027863 EISSN: None Source Type: Journal
DOI: 10.1021/ja8077544 Document Type: Article

Times cited : (32)

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- Experimental procedure: CAUTION! Silver azide is an extremely hazardous and explosive material. All compounds should be handled only on a scale of less than 2 mmol with appropriate safety precautions (safety shields, safety slasses, face shields, leather suits, sloves, and ear plugs, Ignoring these safety precautions can result in serious injury! NMR spectra were recorded at 25 °C on a JEOL Eclipse 400 instrument, and chemical shifts are with respect to MeNO2 (14N, 28.9 MHz, and 2 M AgNO 3/D2O (109Ag, 18.6 MHz, Ph 3S][Ag(N3)2, 1, Into a solution of [Ph 3S]Br (0.29 mmol) in CH3CN (4 mL) was added AgN 3 (0.58 mmol) at ambient temperature. The solution immediately turned red-brownish and a precipitate (AgBr) was obtained. After being stirred for 3 days at ambient temperature, the solution was filtrated, and all volatile materials were removed in vacuo y
- 3 fully characterized incl. X-ray crystallography, submitted for publication.

45
- 67849109396
- Crystal data for 1,C18H15AgN6S: Mr, 455.29, monoclinic, space group Cc, a, 16.3409(12, b, 10.5219(8, c, 10.6388(6) Å, V, 1824.3(2) Å3, F(000, 912, ρcaled (Z, 4, 1.658 g cm-3, μ, 1.234 mm-1, approximate crystal dimensions 0.15 × 0.10 × 0.09 mm3, θ range, 3.8, 26.0°,MoKα (λ, 0.71073 Å, T, 200 K, 8433 measured data (Oxford Xcalibur3 diffractometer with a CCD area detector, of which 3522 (Rint, 0.0447) unique. Structure solution by direct methods, full-matrix least- squares refinement on F2, data to parameters ratio: 15.0:1, final R indices [I > 2δ(I, R1, 0.0370, wR2, 0.0686, R1, 0.0616 (all data, wR2, 0.0796 all data, GOF on F2, 1.041. Further crystallo
- int = 0.0447) unique. Structure solution by direct methods, full-matrix least- squares refinement on F2, data to parameters ratio: 15.0:1, final R indices [I > 2δ(I)]: R1 = 0.0370, wR2 = 0.0686, R1 = 0.0616 (all data), wR2 = 0.0796 (all data), GOF on F2 = 1.041. Further crystallographic details can be obtained from the Cambridge Crystallographic Data Centre (CCDC, 12 Union Road, Cambridge CB21EZ, UK (Fax: (+44) 1223-336-033; e-mail: deposit@ccdc.cam.ac.uk) on quoting the deposition number CSD-692513.

46
- 67849130032
- Crystal data for 2,C24H20AgN6P: Mr, 531.30, monoclinic, space group P2/n, a, 16.4246(7, b, 7.3362, c, 19.1152(8) Å, V, 2242.24(17) Å3, F(000, 1072, ρcaled (Z, 4, 1.574 g cm-3, μ, 0.995 mm-1, approximate crystal dimensions 0.31 × 0.18 × 0.06 mm3, θ range, 3.8- 26.0°,MoKα (λ, 0.71073 Å, T, 135 K, 12464 measured data (Oxford Xcalibur3 diffractometer with a CCD area detector, of which 4383 (Rint, 0.0408) unique. Structure solution by direct methods, full-matrix least- squares refinement on F2, data to parameters ratio: 15.1:1, final R indices [I 7gt; 2δ(I, R1, 0.0308, wR2, 0.0814, R1, 0.0517 (all data, wR2, 0.0885 all data, GOF on F2, 0.981. Further crystallographic
- int = 0.0408) unique. Structure solution by direct methods, full-matrix least- squares refinement on F2, data to parameters ratio: 15.1:1, final R indices [I 7gt; 2δ(I)]: R1 = 0.0308, wR2 = 0.0814, R1 = 0.0517 (all data), wR2 = 0.0885 (all data), GOF on F2 = 0.981. Further crystallographic details can be obtained from the Cambridge Crystallographic Data Centre (CCDC, 12 Union Road, Cambridge CB21EZ, UK (Fax: (+44) 1223-336-033; e-mail: deposit@ccdc.cam.ac.uk) on quoting the deposition number CSD-692514.

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