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MAS NMR under light irradiation is yet little developed, with technical solutions and first applications just emerging. We present the first\n                    <jats:italic>operando<\/jats:italic>\n                    observation of photoreforming of methanol to formaldehyde in a transparent rotor, irradiated at 365\u00a0nm by four LEDs, at spinning rates up to 11.5\u00a0kHz. The photon flux inside the rotor is quantified by an actinometric reaction. Efficient light penetration into the entire rotor volume is crucial. Therefore, we introduce silica monoliths with a continuous network of macropores, coated with TiO\n                    <jats:sub>2<\/jats:sub>\n                    (anatase) as supported heterogeneous catalyst. These monoliths provide a large pore volume to accommodate the liquid substrate and a high surface area. Centrally, the network of pores larger than the visible light enhances light penetration into the material by a factor of two compared to a powder. Silica monoliths may be easily decorated with various photocatalysts and thus provide a versatile platform for observing in real time photocatalytic reactions by solid\u2010state NMR.\n                  <\/jats:p>","DOI":"10.1002\/chem.202503583","type":"journal-article","created":{"date-parts":[[2026,1,21]],"date-time":"2026-01-21T13:20:31Z","timestamp":1769001631000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["<i>Operando<\/i>\n                    Magic Angle Spinning Solid\u2010State NMR Spectroscopy of Methanol Photoreforming Over Titania\u2010Coated Silica Monoliths"],"prefix":"10.1002","volume":"32","author":[{"given":"Fei","family":"Ding","sequence":"first","affiliation":[{"name":"Erlangen Center for Interface Research and Catalysis (ECRC) Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg (FAU)  Erlangen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Karl","family":"K\u00f6nig","sequence":"additional","affiliation":[{"name":"Erlangen Center for Interface Research and Catalysis (ECRC) Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg (FAU)  Erlangen Germany"},{"name":"Faculty For Chemistry and Pharmacy Ludwig\u2010Maximilians\u2010Universit\u00e4t M\u00fcnchen  M\u00fcnchen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Johannes","family":"B\u00f6hmer","sequence":"additional","affiliation":[{"name":"Institute of Micro\u2010 and Nanostructure Research (IMN) &amp; Center for Nanoanalysis and Electron Microscopy (CENEM) Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg (FAU)  Erlangen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Florian M.","family":"Wisser","sequence":"additional","affiliation":[{"name":"Erlangen Center for Interface Research and Catalysis (ECRC) Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg (FAU)  Erlangen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Erdmann","family":"Spiecker","sequence":"additional","affiliation":[{"name":"Institute of Micro\u2010 and Nanostructure Research (IMN) &amp; Center for Nanoanalysis and Electron Microscopy (CENEM) Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg (FAU)  Erlangen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Benjamin Apeleo","family":"Zubiri","sequence":"additional","affiliation":[{"name":"Institute of Micro\u2010 and Nanostructure Research (IMN) &amp; Center for Nanoanalysis and Electron Microscopy (CENEM) Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg (FAU)  Erlangen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3508-3021","authenticated-orcid":false,"given":"Dorothea","family":"Wisser","sequence":"additional","affiliation":[{"name":"Erlangen Center for Interface Research and Catalysis (ECRC) Friedrich\u2010Alexander\u2010Universit\u00e4t Erlangen\u2010N\u00fcrnberg (FAU)  Erlangen Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,1,21]]},"reference":[{"key":"e_1_2_7_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.jpcc.0c05921"},{"key":"e_1_2_7_3_1","doi-asserted-by":"publisher","DOI":"10.1021\/jp9927092"},{"key":"e_1_2_7_4_1","doi-asserted-by":"publisher","DOI":"10.1016\/S0920-5861(98)00449-0"},{"key":"e_1_2_7_5_1","doi-asserted-by":"publisher","DOI":"10.1016\/S0926-2040(03)00030-4"},{"key":"e_1_2_7_6_1","doi-asserted-by":"publisher","DOI":"10.1039\/b315779b"},{"key":"e_1_2_7_7_1","doi-asserted-by":"publisher","DOI":"10.1021\/bi970416y"},{"key":"e_1_2_7_8_1","doi-asserted-by":"publisher","DOI":"10.1039\/D4TA06729K"},{"key":"e_1_2_7_9_1","doi-asserted-by":"publisher","DOI":"10.1073\/pnas.0706156105"},{"key":"e_1_2_7_10_1","doi-asserted-by":"publisher","DOI":"10.1073\/pnas.1507713112"},{"key":"e_1_2_7_11_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.4c06151"},{"key":"e_1_2_7_12_1","doi-asserted-by":"publisher","DOI":"10.1039\/D5TA06364G"},{"key":"e_1_2_7_13_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja992683s"},{"key":"e_1_2_7_14_1","doi-asserted-by":"publisher","DOI":"10.1021\/jp0652289"},{"key":"e_1_2_7_15_1","doi-asserted-by":"publisher","DOI":"10.1006\/jcat.1995.1270"},{"key":"e_1_2_7_16_1","doi-asserted-by":"publisher","DOI":"10.1006\/jcat.1994.1274"},{"key":"e_1_2_7_17_1","doi-asserted-by":"publisher","DOI":"10.1103\/PhysRevLett.107.143901"},{"key":"e_1_2_7_18_1","doi-asserted-by":"publisher","DOI":"10.1038\/srep46637"},{"key":"e_1_2_7_19_1","doi-asserted-by":"publisher","DOI":"10.1364\/OL.35.001740"},{"key":"e_1_2_7_20_1","doi-asserted-by":"publisher","DOI":"10.1039\/D1TA05194F"},{"key":"e_1_2_7_21_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.nanolett.5b01424"},{"key":"e_1_2_7_22_1","doi-asserted-by":"publisher","DOI":"10.1002\/admi.202202131"},{"key":"e_1_2_7_23_1","doi-asserted-by":"publisher","DOI":"10.1107\/S0021889869006868"},{"key":"e_1_2_7_24_1","doi-asserted-by":"publisher","DOI":"10.1039\/c3ra45347b"},{"key":"e_1_2_7_25_1","doi-asserted-by":"publisher","DOI":"10.1088\/0022-3727\/46\/32\/325302"},{"key":"e_1_2_7_26_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja074064m"},{"key":"e_1_2_7_27_1","doi-asserted-by":"publisher","DOI":"10.1103\/PhysRevB.59.6643"},{"key":"e_1_2_7_28_1","doi-asserted-by":"publisher","DOI":"10.1021\/cm0630587"},{"key":"e_1_2_7_29_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemmater.7b02674"},{"key":"e_1_2_7_30_1","doi-asserted-by":"publisher","DOI":"10.1351\/pac200476122105"},{"key":"e_1_2_7_31_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.orglett.8b00391"},{"key":"e_1_2_7_32_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.cattod.2012.08.035"},{"key":"e_1_2_7_33_1","first-page":"115","article-title":"Etude Par Spectroscopie Rmn 13C De la Solution Aqueuse Formaldehyde\u2010methanol","volume":"84","author":"Le Botlan D. 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