{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,5]],"date-time":"2026-10-05T18:36:35Z","timestamp":1791225395321,"version":"4.1.0"},"reference-count":106,"publisher":"Wiley","issue":"3","license":[{"start":{"date-parts":[[2009,11,30]],"date-time":"2009-11-30T00:00:00Z","timestamp":1259539200000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/onlinelibrary.wiley.com\/termsAndConditions#vor"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Chemistry A European J"],"published-print":{"date-parts":[[2010,1,18]]},"abstract":"<jats:title>Abstract<\/jats:title><jats:p>The preparation and characterization of a series of magnesium(II) iodide complexes incorporating \u03b2\u2010diketiminate ligands of varying steric bulk and denticity, namely, [(ArNCMe)<jats:sub>2<\/jats:sub>CH]<jats:sup>\u2212<\/jats:sup> (Ar=phenyl, (<jats:sup>Ph<\/jats:sup>Nacnac), mesityl (<jats:sup>Mes<\/jats:sup>Nacnac), or 2,6\u2010diisopropylphenyl (Dipp, <jats:sup>Dipp<\/jats:sup>Nacnac)), [(DippNC<jats:italic>t<\/jats:italic>Bu)<jats:sub>2<\/jats:sub>CH]<jats:sup>\u2212<\/jats:sup> (<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac), and [(DippNCMe)(Me<jats:sub>2<\/jats:sub>NCH<jats:sub>2<\/jats:sub>CH<jats:sub>2<\/jats:sub>NCMe)CH]<jats:sup>\u2212<\/jats:sup> (<jats:sup>Dmeda<\/jats:sup>Nacnac) are reported. The complexes [(<jats:sup>Ph<\/jats:sup>Nacnac)MgI(OEt<jats:sub>2<\/jats:sub>)], [(<jats:sup>Mes<\/jats:sup>Nacnac)MgI(OEt<jats:sub>2<\/jats:sub>)], [(<jats:sup>Dmeda<\/jats:sup>Nacnac)MgI(OEt<jats:sub>2<\/jats:sub>)], [(<jats:sup>Mes<\/jats:sup>Nacnac)MgI(thf)], [(<jats:sup>Dipp<\/jats:sup>Nacnac)MgI(thf)], [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)MgI], and [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)MgI(DMAP)] (DMAP=4\u2010dimethylaminopyridine) were shown to be monomeric by X\u2010ray crystallography. In addition, the related \u03b2\u2010diketiminato beryllium and calcium iodide complexes, [(<jats:sup>Mes<\/jats:sup>Nacnac)BeI] and [{(<jats:sup>Dipp<\/jats:sup>Nacnac)CaI(OEt<jats:sub>2<\/jats:sub>)}<jats:sub>2<\/jats:sub>] were prepared and crystallographically characterized. The reductions of all metal(II) iodide complexes by using various reagents were attempted. In two cases these reactions led to the magnesium(I) dimers, [(<jats:sup>Mes<\/jats:sup>Nacnac)MgMg(<jats:sup>Mes<\/jats:sup>Nacnac)] and [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)MgMg(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)]. The reduction of a 1:1 mixture of [(<jats:sup>Dipp<\/jats:sup>Nacnac)MgI(OEt<jats:sub>2<\/jats:sub>)] and [(<jats:sup>Mes<\/jats:sup>Nacnac)MgI(OEt<jats:sub>2<\/jats:sub>)] with potassium gave a low yield of the crystallographically characterized complex [(<jats:sup>Dipp<\/jats:sup>Nacnac)Mg(\u03bc\u2010H)(\u03bc\u2010I)Mg(<jats:sup>Mes<\/jats:sup>Nacnac)]. All attempts to form beryllium(I) or calcium(I) dimers by reductions of [(<jats:sup>Mes<\/jats:sup>Nacnac)BeI], [{(<jats:sup>Dipp<\/jats:sup>Nacnac)CaI(OEt<jats:sub>2<\/jats:sub>)}<jats:sub>2<\/jats:sub>], or [{(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)CaI(thf)}<jats:sub>2<\/jats:sub>] have so far been unsuccessful. The further reactivity of the magnesium(I) complexes [(<jats:sup>Mes<\/jats:sup>Nacnac)MgMg(<jats:sup>Mes<\/jats:sup>Nacnac)] and [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)MgMg(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)] towards a variety of Lewis bases and unsaturated organic substrates was explored. These studies led to the complexes [(<jats:sup>Mes<\/jats:sup>Nacnac)Mg(L)Mg(L)(<jats:sup>Mes<\/jats:sup>Nacnac)] (L=THF or DMAP), [(<jats:sup>Mes<\/jats:sup>Nacnac)Mg(\u03bc\u2010AdN<jats:sub>6<\/jats:sub>Ad)Mg(<jats:sup>Mes<\/jats:sup>Nacnac)] (Ad=1\u2010adamantyl), [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)Mg(\u03bc\u2010AdN<jats:sub>6<\/jats:sub>Ad)Mg(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)], and [(<jats:sup>Mes<\/jats:sup>Nacnac)Mg(\u03bc\u2010<jats:italic>t<\/jats:italic>Bu<jats:sub>2<\/jats:sub>N<jats:sub>2<\/jats:sub>C<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>)Mg(<jats:sup>Mes<\/jats:sup>Nacnac)] and revealed that, in general, the reactivity of the magnesium(I) dimers is inversely proportional to their steric bulk. The preparation and characterization of [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)Mg(\u03bc\u2010H)<jats:sub>2<\/jats:sub>Mg(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)] has shown the compound to have different structural and physical properties to [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)MgMg(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)]. Treatment of the former with DMAP has given [(<jats:sup><jats:italic>t<\/jats:italic>Bu<\/jats:sup>Nacnac)Mg(H)(DMAP)], the X\u2010ray crystal structure of which disclosed it to be the first structurally authenticated terminal magnesium hydride complex. Although attempts to prepare [(<jats:sup>Mes<\/jats:sup>Nacnac)Mg(\u03bc\u2010H)<jats:sub>2<\/jats:sub>Mg(<jats:sup>Mes<\/jats:sup>Nacnac)] were not successful, a neutron diffraction study of the corresponding magnesium(I) complex, [(<jats:sup>Mes<\/jats:sup>Nacnac)MgMg(<jats:sup>Mes<\/jats:sup>Nacnac)] confirmed that the compound is devoid of hydride ligands.<\/jats:p>","DOI":"10.1002\/chem.200902425","type":"journal-article","created":{"date-parts":[[2009,11,30]],"date-time":"2009-11-30T15:53:18Z","timestamp":1259596398000},"page":"938-955","source":"Crossref","is-referenced-by-count":452,"title":["\u03b2\u2010Diketiminate\u2010Stabilized Magnesium(I) Dimers and Magnesium(II) Hydride Complexes: Synthesis, Characterization, Adduct Formation, and Reactivity Studies"],"prefix":"10.1002","volume":"16","author":[{"given":"Simon\u2005J.","family":"Bonyhady","sequence":"first","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cameron","family":"Jones","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sharanappa","family":"Nembenna","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Andreas","family":"Stasch","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Alison\u2005J.","family":"Edwards","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Garry\u2005J.","family":"McIntyre","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2010,1,14]]},"reference":[{"key":"e_1_2_6_1_2","unstructured":"Of most relevance to this study is the chemistry of Group\u200513\u201315 element(I) dimers REER (R=bulky aryl alkyl etc. ). 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70\u2005kcal\u2009mol\u22121) than the Mg\uf8ffMg bonds of magnesium(I) dimers RMgMgR (see Ref.\u2005[6])."},{"key":"e_1_2_6_56_2","unstructured":"See the Supporting Information for further details."},{"key":"e_1_2_6_57_2","doi-asserted-by":"publisher","DOI":"10.1016\/j.poly.2005.06.042"},{"key":"e_1_2_6_58_2","doi-asserted-by":"publisher","DOI":"10.1021\/om0202827"},{"key":"e_1_2_6_59_2","doi-asserted-by":"publisher","DOI":"10.1039\/B208679D"},{"key":"e_1_2_6_60_2","unstructured":"Theoretical studies have predicted significantly longer and weaker Ca\uf8ffCa bonds in compounds of the type RCaCaR (Ca\uf8ffCa distances of ca. 3.73\u20133.82\u2005\u00c5; BDEs of<30\u2005kcal\u2009mol\u22121) than the Mg\uf8ffMg bonds of magnesium(I) dimers RMgMgR (see Ref.\u2005[6])."},{"key":"e_1_2_6_61_2","doi-asserted-by":"publisher","DOI":"10.1021\/ar700267b"},{"key":"e_1_2_6_62_2","doi-asserted-by":"publisher","DOI":"10.1039\/C39940001699"},{"key":"e_1_2_6_63_2","unstructured":"A very low yield 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A poor\u2010quality crystal structure of the compound confirmed it to be monomeric in the solid state. No spectroscopic data were obtained. The mechanism of formation of this compound is unknown."},{"key":"e_1_2_6_64_2","unstructured":"The X\u2010ray crystal structure of21 although of low quality ambiguously revealed the connectivity of the compound and showed it to have a similar geometry to that of22."},{"key":"e_1_2_6_65_2","doi-asserted-by":"publisher","DOI":"10.1021\/om050892h"},{"key":"e_1_2_6_66_2","unstructured":"It is of note that the reduction of the unfunctionalized unsaturated substrate 1 3 5 7\u2010cyclooctatetraene by2does occur but only in toluene heated at reflux."},{"key":"e_1_2_6_67_2","doi-asserted-by":"publisher","DOI":"10.1021\/cr50015a001"},{"key":"e_1_2_6_68_2","unstructured":"It is of note that none of the magnesium(I) dimers2 16 or17react with the bulkier carbodiimide DippN=C\uf8feNDipp in toluene at 20\u2009\u00b0C."},{"key":"e_1_2_6_69_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja801375g"},{"key":"e_1_2_6_70_2","unstructured":"See for example:"},{"key":"e_1_2_6_71_2","doi-asserted-by":"publisher","DOI":"10.1021\/jo00342a032"},{"key":"e_1_2_6_72_2","doi-asserted-by":"publisher","DOI":"10.1039\/b416553e"},{"key":"e_1_2_6_73_2","unstructured":"See for example:"},{"key":"e_1_2_6_74_2","doi-asserted-by":"publisher","DOI":"10.1021\/ic061805w"},{"key":"e_1_2_6_75_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0277-5387(97)00487-7"},{"key":"e_1_2_6_76_2","doi-asserted-by":"publisher","DOI":"10.1021\/jp808973e"},{"key":"e_1_2_6_77_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.19901020304"},{"key":"e_1_2_6_77_3","doi-asserted-by":"publisher","DOI":"10.1002\/anie.199002233"},{"key":"e_1_2_6_78_2","doi-asserted-by":"publisher","DOI":"10.1021\/om00042a055"},{"key":"e_1_2_6_79_2","doi-asserted-by":"publisher","DOI":"10.1021\/ic50185a033"},{"key":"e_1_2_6_80_2","doi-asserted-by":"publisher","DOI":"10.1002\/ange.200900878"},{"key":"e_1_2_6_80_3","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200900878"},{"key":"e_1_2_6_81_2","unstructured":"A good yield (76\u2009%) of the related complex [Mg(PhNacnac)2]15can similarly be obtained by treatingPhNacnacH with MgnBu2in hexane at 50\u2009\u00b0C for 20\u2005min."},{"key":"e_1_2_6_82_2","doi-asserted-by":"publisher","DOI":"10.1021\/cr950019y"},{"key":"e_1_2_6_83_2","doi-asserted-by":"publisher","DOI":"10.1039\/b103149j"},{"key":"e_1_2_6_84_2","doi-asserted-by":"publisher","DOI":"10.1016\/j.jorganchem.2005.12.053"},{"key":"e_1_2_6_85_2","doi-asserted-by":"publisher","DOI":"10.1021\/om7010936"},{"key":"e_1_2_6_86_2","doi-asserted-by":"publisher","DOI":"10.1002\/(SICI)1099-0682(199810)1998:10<1485::AID-EJIC1485>3.0.CO;2-F"},{"key":"e_1_2_6_87_2","unstructured":"G.\u2005M. 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