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Unlike the nitrogen analogues CH<jats:sub>3<\/jats:sub>ONO and CH<jats:sub>3<\/jats:sub>NO<jats:sub>2<\/jats:sub>, the experimental data for these two prototypical OPCs are scarce. By high\u2010vacuum flash pyrolysis (HVFP) of the diazide CH<jats:sub>3<\/jats:sub>OP(O)(N<jats:sub>3<\/jats:sub>)<jats:sub>2<\/jats:sub> at 1000\u2005K, the <jats:italic>cis<\/jats:italic> and <jats:italic>trans<\/jats:italic> conformers of CH<jats:sub>3<\/jats:sub>OPO have been generated in the gas phase and subsequently isolated in cryogenic Ar and N<jats:sub>2<\/jats:sub> matrices for IR spectroscopic characterization. Upon 266\u2005nm laser irradiation of CH<jats:sub>3<\/jats:sub>OPO, <jats:italic>cis\u2192trans<\/jats:italic> conformational conversion occurs with concurrent isomerization to CH<jats:sub>3<\/jats:sub>PO<jats:sub>2<\/jats:sub>. The spectroscopic identification of CH<jats:sub>3<\/jats:sub>OPO and CH<jats:sub>3<\/jats:sub>PO<jats:sub>2<\/jats:sub> is supported by D\u2010, <jats:sup>13<\/jats:sup>C\u2010, and <jats:sup>18<\/jats:sup>O\u2010isotope labeling and quantum chemical calculations at the CCSD(T)\u2010F12a\/cc\u2010pVTZ\u2010F12 level using configuration\u2010selective vibrational configuration interaction (VCI).<\/jats:p>","DOI":"10.1002\/anie.201906874","type":"journal-article","created":{"date-parts":[[2019,6,25]],"date-time":"2019-06-25T17:11:46Z","timestamp":1561482706000},"page":"12164-12169","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":33,"title":["Phosphorus Analogues of Methyl Nitrite and Nitromethane: CH<sub>3<\/sub>OPO and CH<sub>3<\/sub>PO<sub>2<\/sub>"],"prefix":"10.1002","volume":"58","author":[{"given":"Xiaofang","family":"Zhao","sequence":"first","affiliation":[{"name":"College of Chemistry Chemical Engineering and Materials 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