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The reaction conditions depend on the substituent R. Alkyl\u2010substituted derivatives (<jats:bold>1\u2009a<\/jats:bold>\u2013<jats:bold>1\u2009d<\/jats:bold>[GaCl<jats:sub>4<\/jats:sub>]) are best synthesized under solvent\u2010free conditions, whereas aryl\u2010substituted derivatives (<jats:bold>1\u2009e<\/jats:bold>\u2013<jats:bold>1\u2009h<\/jats:bold>[GaCl<jats:sub>4<\/jats:sub>]) are formed in C<jats:sub>6<\/jats:sub>H<jats:sub>5<\/jats:sub>F. All compounds have been prepared on a multi\u2010gram scale in good to excellent yields and have been fully characterized with an emphasis on <jats:sup>31<\/jats:sup>P\u2005NMR spectroscopy in solution and single\u2010crystal structure determination. Subsequent chalcogenation reactions of cations R<jats:sub>2<\/jats:sub>P<jats:sub>5<\/jats:sub><jats:sup>+<\/jats:sup> (<jats:bold>1\u2009a<\/jats:bold><jats:sup>+<\/jats:sup>, <jats:bold>1\u2009e<\/jats:bold><jats:sup>+<\/jats:sup>) and trication Ph<jats:sub>6<\/jats:sub>P<jats:sub>7<\/jats:sub><jats:sup>3+<\/jats:sup> (<jats:bold>3<\/jats:bold><jats:sup>3+<\/jats:sup>) with elemental sulfur (\u03b1\u2010S<jats:sub>8<\/jats:sub>) or grey selenium (Se<jats:sub>grey<\/jats:sub>) yielded a series of unique polyphosphorus\u2013chalcogen cations (<jats:bold>4\u2009a<\/jats:bold><jats:sup>+<\/jats:sup>, <jats:bold>4\u2009e<\/jats:bold><jats:sup>+<\/jats:sup>, <jats:bold>5\u2009a<\/jats:bold><jats:sup>+<\/jats:sup>, <jats:bold>6<\/jats:bold><jats:sup>2+<\/jats:sup> and <jats:bold>7<\/jats:bold><jats:sup>2+<\/jats:sup>), possessing nortricyclane\u2010type molecular structures. An in\u2010depth study of the <jats:sup>31<\/jats:sup>P{<jats:sup>1<\/jats:sup>H} and <jats:sup>77<\/jats:sup>Se\u2005NMR spectroscopic parameters is presented, and correlations between the substitution pattern and the observed structural features have been investigated in detail.<\/jats:p>","DOI":"10.1002\/chem.201204337","type":"journal-article","created":{"date-parts":[[2013,6,12]],"date-time":"2013-06-12T08:56:08Z","timestamp":1371027368000},"page":"9895-9907","source":"Crossref","is-referenced-by-count":31,"title":["Synthesis of Cationic R<sub>2<\/sub>P<sub>5<\/sub><sup>+<\/sup> Cages and Subsequent Chalcogenation Reactions"],"prefix":"10.1002","volume":"19","author":[{"given":"Michael H.","family":"Holthausen","sequence":"first","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Alexander","family":"Hepp","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Jan J.","family":"Weigand","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2013,6,12]]},"reference":[{"key":"e_1_2_6_1_2","doi-asserted-by":"publisher","DOI":"10.1002\/asia.200700229"},{"key":"e_1_2_6_2_2","unstructured":"\u00a0"},{"key":"e_1_2_6_3_2","doi-asserted-by":"publisher","DOI":"10.1070\/RC2005v074n09ABEH001182"},{"key":"e_1_2_6_4_2","doi-asserted-by":"publisher","DOI":"10.1021\/cr100010e"},{"key":"e_1_2_6_5_2","doi-asserted-by":"publisher","DOI":"10.1016\/j.ccr.2010.12.016"},{"key":"e_1_2_6_6_2","unstructured":"\u00a0"},{"key":"e_1_2_6_7_2","doi-asserted-by":"publisher","DOI":"10.1002\/1521-3757(20011203)113:23<4544::AID-ANGE4544>3.0.CO;2-C"},{"key":"e_1_2_6_7_3","doi-asserted-by":"publisher","DOI":"10.1002\/1521-3773(20011203)40:23<4406::AID-ANIE4406>3.0.CO;2-X"},{"key":"e_1_2_6_8_2","doi-asserted-by":"publisher","DOI":"10.1002\/1521-3765(20021004)8:19<4475::AID-CHEM4475>3.0.CO;2-M"},{"key":"e_1_2_6_9_2","doi-asserted-by":"publisher","DOI":"10.1039\/b103957c"},{"key":"e_1_2_6_10_2","doi-asserted-by":"publisher","DOI":"10.1002\/chem.200400096"},{"key":"e_1_2_6_11_2","unstructured":"\u00a0"},{"key":"e_1_2_6_12_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja906878q"},{"key":"e_1_2_6_13_2","doi-asserted-by":"publisher","DOI":"10.1039\/c0cc02418j"},{"key":"e_1_2_6_14_2","doi-asserted-by":"publisher","DOI":"10.1002\/zaac.201200123"},{"key":"e_1_2_6_15_2","doi-asserted-by":"publisher","DOI":"10.1021\/ic2013304"},{"key":"e_1_2_6_16_2","unstructured":"\u00a0"},{"key":"e_1_2_6_17_2","doi-asserted-by":"publisher","DOI":"10.1002\/ejic.200800733"},{"key":"e_1_2_6_18_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.200602353"},{"key":"e_1_2_6_18_3","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200602353"},{"key":"e_1_2_6_19_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.200804903"},{"key":"e_1_2_6_19_3","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200804903"},{"key":"e_1_2_6_20_2","doi-asserted-by":"publisher","DOI":"10.1002\/chem.200500138"},{"key":"e_1_2_6_21_2","doi-asserted-by":"publisher","DOI":"10.1002\/1521-3765(20010119)7:2<490::AID-CHEM490>3.0.CO;2-I"},{"key":"e_1_2_6_22_2","doi-asserted-by":"publisher","DOI":"10.1002\/chem.200500142"},{"key":"e_1_2_6_23_2","doi-asserted-by":"publisher","DOI":"10.1021\/om9703595"},{"key":"e_1_2_6_24_2","unstructured":"\u00a0"},{"key":"e_1_2_6_25_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja011075l"},{"key":"e_1_2_6_26_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja036649w"},{"key":"e_1_2_6_27_2","unstructured":"\u00a0"},{"key":"e_1_2_6_28_2","doi-asserted-by":"publisher","DOI":"10.1021\/ic0488738"},{"key":"e_1_2_6_29_2","doi-asserted-by":"publisher","DOI":"10.1039\/C1DT11636C"},{"key":"e_1_2_6_30_2","unstructured":"\u00a0"},{"key":"e_1_2_6_31_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.19820940725"},{"key":"e_1_2_6_31_3","first-page":"544","volume":"21","year":"1982","journal-title":"Angew. 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