Sylwester, Alan P. and Dervan, Peter B. (1984) Low-temperature matrix isolation of the 1,1-diazene H_2NN. Electronic and infrared characterization. Journal of the American Chemical Society, 106 (16). pp. 4648-4650. ISSN 0002-7863. doi:10.1021/ja00328a076. https://resolver.caltech.edu/CaltechAUTHORS:20160511-152019347
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Abstract
We report the photochemical generation of H_2NN (3) in a glass at 80 K and an argon matrix at 10 °K and the isotopically substituted species, D_2NN (3-d_2), H_2N^(15)N (3-^(15)N) and D_2N^(15)N (3-d2, ^(15)N), facilitating the electronic and infrared spectral characterization of 3. Irradiation of carbamoyl azide (4) in a rigid medium (2-methyltetrahydrofuran (2-MTHF) at 80 K) with a 1000-W Xenon lamp through Corning filters CS-7-54 (UV transmitting, visible 440-660 cut-out filters) affords a blue-violet glass. Electronic absorption spectroscopy (80 K) reveals a structured absorption spectrum in the visible (λ_(max) 636 nm) (Figure 1). This is assigned to the n,π* transition for H_2NN. The vibrational progression shows an average spacing of 1300 cm^(-1), presumably the N-N stretching frequency of 81 of H_2NN. Warming the glass to softening (90 °K) results in Joss of the blue-violet species. Irradiation of 4-d_2^(12) affords a similar electronic absorption spectrum.
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Additional Information: | © 1984 American Chemical Society. Received April 13, 1984. We are grateful to the National Science Foundation (CHE-8305790) for support of this research and to the Southern California Regional NMR Facility (NSF Grant 7916324). Contribution No. 7008, Division of Chemistry and Chemical Engineering, California Institute of Technology, Pasadena, California 91125. | ||||||||||||
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Issue or Number: | 16 | ||||||||||||
DOI: | 10.1021/ja00328a076 | ||||||||||||
Record Number: | CaltechAUTHORS:20160511-152019347 | ||||||||||||
Persistent URL: | https://resolver.caltech.edu/CaltechAUTHORS:20160511-152019347 | ||||||||||||
Official Citation: | Low-temperature matrix isolation of the 1,1-diazene H2NN. Electronic and infrared characterization Alan P. Sylwester and Peter B. Dervan Journal of the American Chemical Society 1984 106 (16), 4648-4650 DOI: 10.1021/ja00328a076 | ||||||||||||
Usage Policy: | No commercial reproduction, distribution, display or performance rights in this work are provided. | ||||||||||||
ID Code: | 67021 | ||||||||||||
Collection: | CaltechAUTHORS | ||||||||||||
Deposited By: | Victoria Brennan | ||||||||||||
Deposited On: | 19 May 2016 21:05 | ||||||||||||
Last Modified: | 11 Nov 2021 00:25 |
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