{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,9]],"date-time":"2026-10-09T02:47:58Z","timestamp":1791514078722,"version":"4.3.4"},"reference-count":123,"publisher":"Wiley","issue":"11","license":[{"start":{"date-parts":[[2019,1,29]],"date-time":"2019-01-29T00:00:00Z","timestamp":1548720000000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/onlinelibrary.wiley.com\/termsAndConditions#vor"}],"funder":[{"DOI":"10.13039\/501100001665","name":"Agence Nationale de la Recherche","doi-asserted-by":"publisher","award":["MENOLEP"],"award-info":[{"award-number":["MENOLEP"]}],"id":[{"id":"10.13039\/501100001665","id-type":"DOI","asserted-by":"publisher"}]}],"content-domain":{"domain":["chemistry-europe.onlinelibrary.wiley.com"],"crossmark-restriction":true},"short-container-title":["Chemistry A European J"],"published-print":{"date-parts":[[2019,2,21]]},"abstract":"<jats:title>Abstract<\/jats:title><jats:p>Tame d<jats:sup>0<\/jats:sup> phosphidotitanocene cations stabilized with a pendant tertiary phosphane arm are reported. These compounds were obtained by one\u2010electron oxidation of d<jats:sup>1<\/jats:sup> precursors with [Cp<jats:sub>2<\/jats:sub>Fe][BPh<jats:sub>4<\/jats:sub>]. The electronic structure of these compounds was studied experimentally (EPR, UV\/Vis, and NMR spectroscopy, X\u2010ray diffraction analysis) and through DFT calculations. The theoretical analysis of the bonding situation by using the electron localization function (ELF) shows the presence of \u03c0\u2010interactions between the phosphido ligand and Ti in the d<jats:sup>0<\/jats:sup> complexes, whereas d\u03c0\u2013p\u03c0 repulsion prevents such interactions in the d<jats:sup>1<\/jats:sup> complexes. In addition, CH\u2013\u03c0 interactions were observed in several complexes, both in solution and in the solid state, between the phosphido ligand and the phosphane arm. The d<jats:sup>0<\/jats:sup> complexes were found to be light sensitive, and decompose through Ti\u2212P bond homolysis to give Ti<jats:sup>III<\/jats:sup> species. A naked d<jats:sup>0<\/jats:sup> phosphidotitanocene cation has been trapped by reaction with diphenylacetylene, yielding a Ti\/P frustrated Lewis pair (FLP), which was found to be less reactive than a previously reported Zr analog.<\/jats:p>","DOI":"10.1002\/chem.201805430","type":"journal-article","created":{"date-parts":[[2018,12,3]],"date-time":"2018-12-03T04:24:55Z","timestamp":1543811095000},"page":"2803-2815","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":15,"title":["The Taming of Redox\u2010Labile Phosphidotitanocene Cations"],"prefix":"10.1002","volume":"25","author":[{"given":"Adrien T.","family":"Normand","sequence":"first","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Quentin","family":"Bonnin","sequence":"additional","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"St\u00e9phane","family":"Brand\u00e8s","sequence":"additional","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Philippe","family":"Richard","sequence":"additional","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3114-2522","authenticated-orcid":false,"given":"Paul","family":"Fleurat\u2010Lessard","sequence":"additional","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Charles H.","family":"Devillers","sequence":"additional","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"C\u00e9dric","family":"Balan","sequence":"additional","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pierre","family":"Le\u2005Gendre","sequence":"additional","affiliation":[{"name":"ICMUB, UMR CNRS 6302 Universit\u00e9 de Bourgogne, UFR sciences et techniques, 9 rue Alain Savary-BP 47870  21078 Dijon Cedex France"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gerald","family":"Kehr","sequence":"additional","affiliation":[{"name":"Organisch-Chemisches Institut Universit\u00e4t M\u00fcnster  Corrensstrasse 40 48149 M\u00fcnster Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gerhard","family":"Erker","sequence":"additional","affiliation":[{"name":"Organisch-Chemisches Institut Universit\u00e4t M\u00fcnster  Corrensstrasse 40 48149 M\u00fcnster Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2019,1,29]]},"reference":[{"key":"e_1_2_7_1_1","unstructured":"\u00a0"},{"key":"e_1_2_7_2_2","doi-asserted-by":"publisher","DOI":"10.1002\/cber.19640970313"},{"key":"e_1_2_7_3_2","doi-asserted-by":"publisher","DOI":"10.1515\/znb-1966-0604"},{"key":"e_1_2_7_4_1","unstructured":"For reviews see:"},{"key":"e_1_2_7_5_2","doi-asserted-by":"publisher","DOI":"10.1021\/cr00030a009"},{"key":"e_1_2_7_6_2","doi-asserted-by":"publisher","DOI":"10.1002\/(SICI)1521-3773(20000117)39:2<314::AID-ANIE314>3.0.CO;2-D"},{"key":"e_1_2_7_6_3","doi-asserted-by":"publisher","DOI":"10.1002\/(SICI)1521-3757(20000117)112:2<322::AID-ANGE322>3.0.CO;2-6"},{"key":"e_1_2_7_7_2","doi-asserted-by":"publisher","DOI":"10.1039\/B813332H"},{"key":"e_1_2_7_8_2","doi-asserted-by":"publisher","DOI":"10.1016\/j.ccr.2011.12.014"},{"key":"e_1_2_7_9_1","unstructured":"See refs.\u20051 2 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was first observed by Issleib in 1964 see ref.\u2005[1a]. In this case further reduction of [TiCl4(2\u2009THF)] to TiIIgave the intriguing homoleptic complex [Ti(PCy2)2]."},{"key":"e_1_2_7_64_1","unstructured":"The phosphinyl radical then recombines to form a diphosphane (R2P-PR2)."},{"key":"e_1_2_7_65_1","unstructured":"See ref.\u2005[4e] and"},{"key":"e_1_2_7_66_2","doi-asserted-by":"publisher","DOI":"10.1002\/zaac.19693700510"},{"key":"e_1_2_7_67_1","unstructured":"Cationic d0phosphidotitanocene complexes [Cp2TiP(SiMe3)2]+and [Cp2Ti(PPh2)(PMe3)]+have previously been envisaged from a theoretical perspective:"},{"key":"e_1_2_7_68_2","doi-asserted-by":"publisher","DOI":"10.1016\/0009-2614(91)87125-U"},{"key":"e_1_2_7_69_2","doi-asserted-by":"publisher","DOI":"10.1021\/ic00092a015"},{"key":"e_1_2_7_70_1","unstructured":"\u00a0"},{"key":"e_1_2_7_71_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0022-328X(01)01248-7"},{"key":"e_1_2_7_72_2","doi-asserted-by":"publisher","DOI":"10.1021\/acs.organomet.5b00250"},{"key":"e_1_2_7_73_1","unstructured":"The first equivalent of phosphide acts as a sacrificial reductant generating R2P-PR2as a byproduct."},{"key":"e_1_2_7_74_1","doi-asserted-by":"publisher","DOI":"10.1021\/ja00423a017"},{"key":"e_1_2_7_75_1","unstructured":"As noted elsewhere in the case of amidoziroconcene cations (ref.\u2005[7a]) the lone pair of phosphorus would have to be in the equatorial plane of the bent Cp2M fragment for \u03c0-interactions to occur."},{"key":"e_1_2_7_76_1","doi-asserted-by":"publisher","DOI":"10.1039\/b801115j"},{"key":"e_1_2_7_77_1","unstructured":"\u00a0"},{"key":"e_1_2_7_78_2","doi-asserted-by":"publisher","DOI":"10.1039\/b902318f"},{"key":"e_1_2_7_79_2","doi-asserted-by":"publisher","DOI":"10.1039\/b313104a"},{"key":"e_1_2_7_80_1","unstructured":"\u00a0"},{"key":"e_1_2_7_81_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0968-0896(98)00002-9"},{"key":"e_1_2_7_82_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201309371"},{"key":"e_1_2_7_82_3","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201309371"},{"key":"e_1_2_7_83_1","unstructured":"To circumvent hydrolysis by residual water measurements were conducted with 10\u22122\u2009msolutions of the complexes in 0.1\u2005mm cells."},{"key":"e_1_2_7_84_1","unstructured":"\u00a0"},{"key":"e_1_2_7_85_2","volume-title":"Time-Dependent Density Functional Theory: A Tool to Explore Excited States, in Handbook of Computational Chemistry","author":"Escudero D.","year":"2015"},{"key":"e_1_2_7_86_2","doi-asserted-by":"publisher","DOI":"10.1021\/acs.jctc.5b01219"},{"key":"e_1_2_7_87_1","unstructured":"\u00a0"},{"key":"e_1_2_7_88_2","doi-asserted-by":"publisher","DOI":"10.1021\/om00026a036"},{"key":"e_1_2_7_89_2","doi-asserted-by":"publisher","DOI":"10.1021\/om960918s"},{"key":"e_1_2_7_90_1","unstructured":"We have previously used phi as an indicator of \u03c0-interactions between Zr and N or P in zirconocene complexes see ref.\u2005[7a]."},{"key":"e_1_2_7_91_1","unstructured":"It is interesting to note that a clear \u03c0-interaction was found by Alhrichs in the TiIII[Cp2TiP(SiMe3)2] complex (ref.\u2005[12a]). The Ti\u2013P \u03c0-interaction in this complex is possible because the metallocene fragment is supported only by the phosphide ligand: therefore the single electron on titanium and the p\u03c0 electrons on phosphorus occupy orthogonal orbitals. This is no longer possible in complexes2in which the titanium atom is tetracoordinated: all d orbitals are involved in bonds and the single electron is bound to interact with the lone pair of the phosphido ligand. This leads to a bent geometry a classical situation in phosphido ligand chemistry (see ref.\u2005[2d])."},{"key":"e_1_2_7_92_1","unstructured":"1H\u2005NMR signals were assigned unambiguously through1H-13C correlation experiments that is HSQC and HMBC. Also the31P spectrum of3\u2009bshows that the hydrogens on C11 couple with P1 not P2. See the Supporting Information."},{"key":"e_1_2_7_93_1","first-page":"7","volume-title":"The Range of Chemical Shifts, Coupling Constants, and What Influences Each, in Phosphorus-31 NMR Spectroscopy: A Concise Introduction for the Synthetic Organic and Organometallic Chemist","author":"K\u00fchl O.","year":"2008"},{"key":"e_1_2_7_94_1","doi-asserted-by":"publisher","DOI":"10.1039\/c1nj20292h"},{"key":"e_1_2_7_95_1","unstructured":"The exact chemical shift could not be ascertained owing to multiple overlaps in the1H\u2005NMR spectrum of3\u2009d."},{"key":"e_1_2_7_96_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.5b12597"},{"key":"e_1_2_7_97_1","unstructured":"We also observed small intensity (\u03f5=2210\u20133220\u2005cm\u22121\u2009m\u22121) shouldering bands in the UV region (3\u2009b: 348\u2005nm;3\u2009c: 342\u2005nm;3\u2009d: 346\u2005nm) although we were unable to assign them through DFT calculations."},{"key":"e_1_2_7_98_1","unstructured":"Although the absence of (PCy2)2is surprising in the case of3\u2009f it could just be that the presence of PCy2H in the reaction mixture prevents the phosphinyl radical from dimerizing instead promoting other termination pathways for example H abstraction from the solvent."},{"key":"e_1_2_7_99_1","unstructured":"ComplexEwas characterized in C6D5Br at 299\u2005K see ref.\u2005[7a]."},{"key":"e_1_2_7_100_1","unstructured":"\u00a0"},{"key":"e_1_2_7_101_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja00309a049"},{"key":"e_1_2_7_102_2","doi-asserted-by":"publisher","DOI":"10.1021\/j100152a020"},{"key":"e_1_2_7_103_2","doi-asserted-by":"publisher","DOI":"10.1021\/ma9810666"},{"key":"e_1_2_7_104_1","doi-asserted-by":"publisher","DOI":"10.1039\/C3SC52327F"},{"key":"e_1_2_7_105_1","unstructured":"See compound10\u2009a\u2032in ref.\u2005[7a]."},{"key":"e_1_2_7_106_1","unstructured":"Gaussian\u200509 Revision\u2005D.01 M.\u2005J. Frisch G.\u2005W. Trucks H.\u2005B. Schlegel G.\u2005E. Scuseria M.\u2005A. Robb J.\u2005R. Cheeseman G. Scalmani V. Barone B. Mennucci G.\u2005A. Petersson H. Nakatsuji M. Caricato X. Li H.\u2005P. Hratchian A.\u2005F. Izmaylov J. Bloino G. Zheng J.\u2005L. Sonnenberg M. Hada M. Ehara K. Toyota R. Fukuda J. Hasegawa M. Ishida T. Nakajima Y. Honda O. Kitao H. Nakai T. Vreven J.\u2005A. Montgomery Jr. J.\u2005E. Peralta F. Ogliaro M. Bearpark J.\u2005J. Heyd E. Brothers K.\u2005N. Kudin V.\u2005N. Staroverov R. Kobayashi J. Normand K. Raghavachari A. Rendell J.\u2005C. Burant S.\u2005S. Iyengar J. Tomasi M. Cossi N. Rega J.\u2005M. Millam M. Klene J.\u2005E. Knox J.\u2005B. Cross V. Bakken C. Adamo J. Jaramillo R. Gomperts R.\u2005E. Stratmann O. Yazyev A.\u2005J. Austin R. Cammi C. Pomelli J.\u2005W. Ochterski R.\u2005L. Martin K. Morokuma V.\u2005G. Zakrzewski G.\u2005A. Voth P. Salvador J.\u2005J. Dannenberg S. Dapprich A.\u2005D. Daniels \u00d6. Farkas J.\u2005B. Foresman J.\u2005V. Ortiz J. Cioslowski D.\u2005J. Fox Gaussian Inc. Wallingford CT 2009."},{"key":"e_1_2_7_107_1","unstructured":"\u00a0"},{"key":"e_1_2_7_108_2","doi-asserted-by":"publisher","DOI":"10.1039\/b515623h"},{"key":"e_1_2_7_109_2","doi-asserted-by":"publisher","DOI":"10.1039\/b508541a"},{"key":"e_1_2_7_110_1","unstructured":"\u00a0"},{"key":"e_1_2_7_111_2","doi-asserted-by":"publisher","DOI":"10.1021\/jp020124t"},{"key":"e_1_2_7_112_2","doi-asserted-by":"publisher","DOI":"10.1021\/cr9904009"},{"key":"e_1_2_7_113_1","doi-asserted-by":"publisher","DOI":"10.1016\/0263-7855(96)00018-5"},{"key":"e_1_2_7_114_1","doi-asserted-by":"publisher","DOI":"10.1063\/1.1558471"},{"key":"e_1_2_7_115_1","doi-asserted-by":"publisher","DOI":"10.1039\/b905554a"},{"key":"e_1_2_7_116_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.inorgchem.6b02510"},{"key":"e_1_2_7_117_1","unstructured":"\u00a0"},{"key":"e_1_2_7_118_2","doi-asserted-by":"publisher","DOI":"10.1021\/ct100466k"},{"key":"e_1_2_7_119_2","doi-asserted-by":"publisher","DOI":"10.1063\/1.1998907"},{"key":"e_1_2_7_120_1","first-page":"165","volume-title":"The IGLO-Method: Ab-initio Calculation and Interpretation of NMR Chemical Shifts and Magnetic Susceptibilities, in Deuterium and Shift Calculation,","author":"Kutzelnigg W.","year":"1990"},{"key":"e_1_2_7_121_1","unstructured":"https:\/\/bse.pnl.gov\/bse\/portal accessed 04\/05\/2016."}],"container-title":["Chemistry \u2013 A European Journal"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/api.wiley.com\/onlinelibrary\/tdm\/v1\/articles\/10.1002%2Fchem.201805430","content-type":"application\/pdf","content-version":"vor","intended-application":"text-mining"},{"URL":"https:\/\/onlinelibrary.wiley.com\/doi\/pdf\/10.1002\/chem.201805430","content-type":"application\/pdf","content-version":"vor","intended-application":"text-mining"},{"URL":"https:\/\/onlinelibrary.wiley.com\/doi\/full-xml\/10.1002\/chem.201805430","content-type":"application\/xml","content-version":"vor","intended-application":"text-mining"},{"URL":"https:\/\/chemistry-europe.onlinelibrary.wiley.com\/doi\/pdf\/10.1002\/chem.201805430","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,12]],"date-time":"2025-10-12T15:54:10Z","timestamp":1760284450000},"score":1,"resource":{"primary":{"URL":"https:\/\/chemistry-europe.onlinelibrary.wiley.com\/doi\/10.1002\/chem.201805430"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2019,1,29]]},"references-count":123,"journal-issue":{"issue":"11","published-print":{"date-parts":[[2019,2,21]]}},"alternative-id":["10.1002\/chem.201805430"],"URL":"https:\/\/doi.org\/10.1002\/chem.201805430","archive":["Portico"],"relation":{},"ISSN":["0947-6539","1521-3765"],"issn-type":[{"value":"0947-6539","type":"print"},{"value":"1521-3765","type":"electronic"}],"subject":[],"published":{"date-parts":[[2019,1,29]]},"assertion":[{"value":"2018-10-30","order":0,"name":"received","label":"Received","group":{"name":"publication_history","label":"Publication History"}},{"value":"2019-01-29","order":3,"name":"published","label":"Published","group":{"name":"publication_history","label":"Publication History"}}]}}