{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,1,24]],"date-time":"2026-01-24T01:55:49Z","timestamp":1769219749450,"version":"3.49.0"},"reference-count":18,"publisher":"International Union of Crystallography (IUCr)","issue":"5","license":[{"start":{"date-parts":[[2019,4,9]],"date-time":"2019-04-09T00:00:00Z","timestamp":1554768000000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/journals.iucr.org\/services\/copyrightpolicy.html"},{"start":{"date-parts":[[2019,4,9]],"date-time":"2019-04-09T00:00:00Z","timestamp":1554768000000},"content-version":"tdm","delay-in-days":0,"URL":"http:\/\/journals.iucr.org\/services\/copyrightpolicy.html#TDM"}],"funder":[{"DOI":"10.13039\/100000928","name":"The Welch Foundation","doi-asserted-by":"crossref","award":["R-0021"],"award-info":[{"award-number":["R-0021"]}],"id":[{"id":"10.13039\/100000928","id-type":"DOI","asserted-by":"crossref"}]}],"content-domain":{"domain":["iucr.org","wiley.com","iucrj.org"],"crossmark-restriction":true},"short-container-title":["Acta Crystallogr C Struct Chem","Acta Crystallogr C","Acta Crystallogr C Cryst Struct Commun","Acta Cryst C","Acta Cryst C Struct Chem","Acta Cryst Sect C","Acta Cryst Sect C Struct Chem","Acta Crystallogr Sect C","Acta Crystallogr Sect C Struct Chem","Acta Crystallogr Sect C Cryst Struct Commun"],"accepted":{"date-parts":[[2019,3,28]]},"published-print":{"date-parts":[[2019,5,1]]},"abstract":"<jats:p>Three asymmetric diosmium(I) carbonyl sawhorse complexes have been prepared by microwave heating. One of these complexes is of the type Os<jats:sub>2<\/jats:sub>(\u03bc-O<jats:sub>2<\/jats:sub>C<jats:italic>R<\/jats:italic>)(\u03bc-O<jats:sub>2<\/jats:sub>C<jats:italic>R<\/jats:italic>\u2032)(CO)<jats:sub>4<\/jats:sub>\n                  <jats:italic>L<\/jats:italic>\n                  <jats:sub>2<\/jats:sub>, with two different bridging carboxylate ligands, while the other two complexes are of the type Os<jats:sub>2<\/jats:sub>(\u03bc-O<jats:sub>2<\/jats:sub>C<jats:italic>R<\/jats:italic>)<jats:sub>2<\/jats:sub>(CO)<jats:sub>5<\/jats:sub>\n                  <jats:italic>L<\/jats:italic>, with one axial CO ligand and one axial phosphane ligand. The mixed carboxylate complex Os<jats:sub>2<\/jats:sub>(\u03bc-acetate)(\u03bc-propionate)(CO)<jats:sub>4<\/jats:sub>[P(<jats:italic>p<\/jats:italic>-tolyl)<jats:sub>3<\/jats:sub>]<jats:sub>2<\/jats:sub>, (<jats:bold>1<\/jats:bold>), was prepared by heating Os<jats:sub>3<\/jats:sub>(CO)<jats:sub>12<\/jats:sub> with a mixture of acetic and propionic acids, isolating Os<jats:sub>2<\/jats:sub>(\u03bc-acetate)(\u03bc-propionate)(CO)<jats:sub>6<\/jats:sub>, and then replacing two CO ligands with two phosphane ligands. This is the first example of an Os<jats:sub>2<\/jats:sub> sawhorse complex with two different carboxylate bridges. The syntheses of Os<jats:sub>2<\/jats:sub>(\u03bc-acetate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>5<\/jats:sub>[P(<jats:italic>p<\/jats:italic>-tolyl)<jats:sub>3<\/jats:sub>], (<jats:bold>3<\/jats:bold>), and Os<jats:sub>2<\/jats:sub>(\u03bc-propionate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>5<\/jats:sub>[P(<jats:italic>p<\/jats:italic>-tolyl)<jats:sub>3<\/jats:sub>], (<jats:bold>6<\/jats:bold>), involved the reaction of Os<jats:sub>3<\/jats:sub>(CO)<jats:sub>12<\/jats:sub> with the appropriate carboxylic acid to initially produce Os<jats:sub>2<\/jats:sub>(\u03bc-carboxylate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>6<\/jats:sub>, followed by treatment with refluxing tetrahydrofuran (THF) to form Os<jats:sub>2<\/jats:sub>(\u03bc-carboxylate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>5<\/jats:sub>(THF), and finally addition of tri-<jats:italic>p<\/jats:italic>-tolylphosphane to replace the THF ligand with the P(<jats:italic>p<\/jats:italic>-tolyl)<jats:sub>3<\/jats:sub> ligand. Neutral complexes of the type Os<jats:sub>2<\/jats:sub>(\u03bc-O<jats:sub>2<\/jats:sub>C<jats:italic>R<\/jats:italic>)<jats:sub>2<\/jats:sub>(CO)<jats:sub>5<\/jats:sub>\n                  <jats:italic>L<\/jats:italic> had not previously been subjected to X-ray crystallographic analysis. The more symmetrical disubstituted complexes, <jats:italic>i.e.<\/jats:italic> Os<jats:sub>2<\/jats:sub>(\u03bc-formate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>4<\/jats:sub>[P(<jats:italic>p<\/jats:italic>-tolyl)<jats:sub>3<\/jats:sub>]<jats:sub>2<\/jats:sub>, (<jats:bold>8<\/jats:bold>), Os<jats:sub>2<\/jats:sub>(\u03bc-acetate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>4<\/jats:sub>[P(<jats:italic>p<\/jats:italic>-tolyl)<jats:sub>3<\/jats:sub>]<jats:sub>2<\/jats:sub>, (<jats:bold>4<\/jats:bold>), and Os<jats:sub>2<\/jats:sub>(\u03bc-propionate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>4<\/jats:sub>[P(<jats:italic>p<\/jats:italic>-tolyl)<jats:sub>3<\/jats:sub>]<jats:sub>2<\/jats:sub>, (<jats:bold>7<\/jats:bold>), as well as the previously reported symmetrical unsubstituted complexes Os<jats:sub>2<\/jats:sub>(\u03bc-acetate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>6<\/jats:sub>, (<jats:bold>2<\/jats:bold>), and Os<jats:sub>2<\/jats:sub>(\u03bc-propionate)<jats:sub>2<\/jats:sub>(CO)<jats:sub>6<\/jats:sub>, (<jats:bold>5<\/jats:bold>), were also prepared in order to examine the influence of axial ligand substitution on the Os\u2014Os bond distance in these sawhorse molecules. Eight crystal structures have been determined and studied, namely \u03bc-acetato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032-\u03bc-propanoato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032-bis[tris(4-methylphenyl)phosphane]-1\u03ba<jats:italic>P<\/jats:italic>,2\u03ba<jats:italic>P<\/jats:italic>\u2032-bis(dicarbonylosmium)(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>) dichloromethane monosolvate, [Os<jats:sub>2<\/jats:sub>(C<jats:sub>2<\/jats:sub>H<jats:sub>3<\/jats:sub>O<jats:sub>2<\/jats:sub>)(C<jats:sub>3<\/jats:sub>H<jats:sub>5<\/jats:sub>O<jats:sub>2<\/jats:sub>)(C<jats:sub>21<\/jats:sub>H<jats:sub>21<\/jats:sub>P)<jats:sub>2<\/jats:sub>(CO)<jats:sub>4<\/jats:sub>]\u00b7CH<jats:sub>2<\/jats:sub>Cl<jats:sub>2<\/jats:sub>, (<jats:bold>1<\/jats:bold>), bis(\u03bc-acetato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032)bis(tricarbonylosmium)(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>), [Os<jats:sub>2<\/jats:sub>(C<jats:sub>2<\/jats:sub>H<jats:sub>3<\/jats:sub>O<jats:sub>2<\/jats:sub>)<jats:sub>2<\/jats:sub>(CO)<jats:sub>6<\/jats:sub>], (<jats:bold>2<\/jats:bold>) (redetermined structure), bis(\u03bc-acetato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032)pentacarbonyl-1\u03ba<jats:sup>2<\/jats:sup>\n                  <jats:italic>C<\/jats:italic>,2\u03ba<jats:sup>3<\/jats:sup>\n                  <jats:italic>C<\/jats:italic>-[tris(4-methylphenyl)phosphane-1\u03ba<jats:italic>P<\/jats:italic>]diosmium(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>), [Os<jats:sub>2<\/jats:sub>(C<jats:sub>2<\/jats:sub>H<jats:sub>3<\/jats:sub>O<jats:sub>2<\/jats:sub>)<jats:sub>2<\/jats:sub>(C<jats:sub>21<\/jats:sub>H<jats:sub>21<\/jats:sub>P)(CO)<jats:sub>5<\/jats:sub>], (<jats:bold>3<\/jats:bold>), bis(\u03bc-acetato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032)bis[tris(4-methylphenyl)phosphane]-1\u03ba<jats:italic>P<\/jats:italic>,2\u03ba<jats:italic>P<\/jats:italic>-bis(dicarbonylosmium)(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>) <jats:italic>p<\/jats:italic>-xylene sesquisolvate, [Os<jats:sub>2<\/jats:sub>(C<jats:sub>2<\/jats:sub>H<jats:sub>3<\/jats:sub>O<jats:sub>2<\/jats:sub>)<jats:sub>2<\/jats:sub>(C<jats:sub>21<\/jats:sub>H<jats:sub>21<\/jats:sub>P)<jats:sub>2<\/jats:sub>(CO)<jats:sub>4<\/jats:sub>]\u00b71.5C<jats:sub>8<\/jats:sub>H<jats:sub>10<\/jats:sub>, (<jats:bold>4<\/jats:bold>), bis(\u03bc-propanoato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032)bis(tricarbonylosmium)(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>), [Os<jats:sub>2<\/jats:sub>(C<jats:sub>3<\/jats:sub>H<jats:sub>5<\/jats:sub>O<jats:sub>2<\/jats:sub>)<jats:sub>2<\/jats:sub>(CO)<jats:sub>6<\/jats:sub>], (<jats:bold>5<\/jats:bold>), pentacarbonyl-1\u03ba<jats:sup>2<\/jats:sup>\n                  <jats:italic>C<\/jats:italic>,2\u03ba<jats:sup>3<\/jats:sup>\n                  <jats:italic>C<\/jats:italic>-bis(\u03bc-propanoato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032)[tris(4-methylphenyl)phosphane-1\u03ba<jats:italic>P<\/jats:italic>]diosmium(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>), [Os<jats:sub>2<\/jats:sub>(C<jats:sub>3<\/jats:sub>H<jats:sub>5<\/jats:sub>O<jats:sub>2<\/jats:sub>)<jats:sub>2<\/jats:sub>(C<jats:sub>21<\/jats:sub>H<jats:sub>21<\/jats:sub>P)(CO)<jats:sub>5<\/jats:sub>], (<jats:bold>6<\/jats:bold>), bis(\u03bc-propanoato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032)bis[tris(4-methylphenyl)phosphane]-1\u03ba<jats:italic>P<\/jats:italic>,2\u03ba<jats:italic>P<\/jats:italic>-bis(dicarbonylosmium)(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>) dichloromethane monosolvate, [Os<jats:sub>2<\/jats:sub>(C<jats:sub>3<\/jats:sub>H<jats:sub>5<\/jats:sub>O<jats:sub>2<\/jats:sub>)<jats:sub>2<\/jats:sub>(C<jats:sub>21<\/jats:sub>H<jats:sub>21<\/jats:sub>P)<jats:sub>2<\/jats:sub>(CO)<jats:sub>4<\/jats:sub>]\u00b7CH<jats:sub>2<\/jats:sub>Cl<jats:sub>2<\/jats:sub>, (<jats:bold>7<\/jats:bold>), and bis(\u03bc-formato-1\u03ba<jats:italic>O<\/jats:italic>:2\u03ba<jats:italic>O<\/jats:italic>\u2032)bis[tris(4-methylphenyl)phosphane]-1\u03ba<jats:italic>P<\/jats:italic>,2\u03ba<jats:italic>P<\/jats:italic>-bis(dicarbonylosmium)(<jats:italic>Os<\/jats:italic>\u2014<jats:italic>Os<\/jats:italic>), [Os<jats:sub>2<\/jats:sub>(CHO<jats:sub>2<\/jats:sub>)<jats:sub>2<\/jats:sub>(C<jats:sub>21<\/jats:sub>H<jats:sub>21<\/jats:sub>P)<jats:sub>2<\/jats:sub>(CO)<jats:sub>4<\/jats:sub>], (<jats:bold>8<\/jats:bold>).<\/jats:p>","DOI":"10.1107\/s2053229619004236","type":"journal-article","created":{"date-parts":[[2019,4,9]],"date-time":"2019-04-09T17:02:32Z","timestamp":1554829352000},"page":"529-537","update-policy":"https:\/\/doi.org\/10.1107\/cm_01","source":"Crossref","is-referenced-by-count":8,"title":["Asymmetric diosmium sawhorse complexes"],"prefix":"10.1107","volume":"75","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-1051-6516","authenticated-orcid":true,"given":"Kylie 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