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A comparison of the spectra with those of the corresponding free B\/P FLPs shows that both <jats:sup>11<\/jats:sup>B isotropic chemical shifts as well as nuclear electric quadrupolar coupling constants decrease significantly upon FLP hydrogenation, revealing the breakage of the partial B\u2212P bond present in the starting materials. Likewise, the <jats:sup>31<\/jats:sup>P isotropic chemical shift, the chemical shift anisotropy, and the asymmetry parameter decrease significantly upon FLP hydrogenation, reflecting the formation of a more symmetric, C<jats:sub>3v<\/jats:sub>\u2010like local environment. <jats:sup>11<\/jats:sup>B{<jats:sup>31<\/jats:sup>P} rotational echo double resonance (REDOR) experiments can be used to measure the B\u2212P internuclear distance (about 3.2\u2005\u00c5) of these compounds. Observation of the hydrogen atoms bound to the Lewis centers is best accomplished via <jats:sup>31<\/jats:sup>P{<jats:sup>1<\/jats:sup>H} and <jats:sup>11<\/jats:sup>B{<jats:sup>1<\/jats:sup>H} cross\u2010polarization\u2010heteronuclear correlation experiments or by direct observation of the <jats:sup>2<\/jats:sup>H MAS NMR signals on especially prepared FLP\u2010D<jats:sub>2<\/jats:sub> adducts. For accurately measuring the phosphorus\u2010deuterium distance via <jats:sup>31<\/jats:sup>P{<jats:sup>2<\/jats:sup>H} rotational echo adiabatic passage double resonance (REAPDOR), it is essential to take the secondary dipolar coupling of <jats:sup>31<\/jats:sup>P with the boron\u2010bonded <jats:sup>2<\/jats:sup>H nuclei explicitly into consideration, by simulating a <jats:sup>2<\/jats:sup>H<jats:sub>P<\/jats:sub>\u2010<jats:sup>31<\/jats:sup>P\u2010<jats:sup>2<\/jats:sup>H<jats:sub>B<\/jats:sub> three\u2010spin system based on structural input. All of the experimental NMR interaction parameters are found in excellent agreement with values calculated by DFT methods, using the geometries obtained either by energy optimization or from single\u2010crystal structures.<\/jats:p>","DOI":"10.1002\/cphc.201900406","type":"journal-article","created":{"date-parts":[[2019,5,24]],"date-time":"2019-05-24T21:54:37Z","timestamp":1558734877000},"page":"1837-1849","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["Dihydrogen Splitting by Intramolecular Borane\u2010Phosphane Frustrated Lewis Pairs: A Comprehensive Characterization Strategy Using Solid State NMR and DFT Calculations"],"prefix":"10.1002","volume":"20","author":[{"given":"Robert","family":"Knitsch","sequence":"first","affiliation":[{"name":"Institut f\u00fcr Physikalische Chemie WWU M\u00fcnster  Corrensstra\u00dfe 30 D-41849 M\u00fcnster Germany"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Thomas","family":"\u00d6zg\u00fcn","sequence":"additional","affiliation":[{"name":"Organisch-Chemisches Institut WWU M\u00fcnster  Corrensstra\u00dfe 40 D-41849 M\u00fcnster Germany"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Guo\u2010Qiang","family":"Chen","sequence":"additional","affiliation":[{"name":"Organisch-Chemisches Institut WWU M\u00fcnster  Corrensstra\u00dfe 40 D-41849 M\u00fcnster Germany"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Gerald","family":"Kehr","sequence":"additional","affiliation":[{"name":"Organisch-Chemisches Institut WWU M\u00fcnster  Corrensstra\u00dfe 40 D-41849 M\u00fcnster Germany"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Gerhard","family":"Erker","sequence":"additional","affiliation":[{"name":"Organisch-Chemisches Institut WWU M\u00fcnster  Corrensstra\u00dfe 40 D-41849 M\u00fcnster Germany"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Michael Ryan","family":"Hansen","sequence":"additional","affiliation":[{"name":"Institut f\u00fcr Physikalische Chemie WWU M\u00fcnster  Corrensstra\u00dfe 30 D-41849 M\u00fcnster Germany"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6536-0117","authenticated-orcid":false,"given":"Hellmut","family":"Eckert","sequence":"additional","affiliation":[{"name":"Institut f\u00fcr Physikalische Chemie WWU M\u00fcnster  Corrensstra\u00dfe 30 D-41849 M\u00fcnster Germany"},{"name":"Instituto de F\u00edsica de S\u00e3o Carlos Universidade de S\u00e3o Paulo  S\u00e3o Carlos SP 13566\u2013590 Brazil"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2019,6,21]]},"reference":[{"key":"e_1_2_7_1_1","first-page":"1","volume-title":"Frustrated Lewis Pairs I: Uncovering and Understanding","author":"Stephan D. 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