Synthesis and Structure of the Dimethyl Sulfide Complexes [OsX 4 (dms) 2 ] (Х = Cl, Br) and [Os 2 OCl 6 (dms) 4 ]

Synthesis and Structure of the Dimethyl Sulfide Complexes [OsX 4 (dms) 2 ] (Х = Cl, Br) and [Os 2 OCl 6 (dms) 4 ] | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Synthesis and Structure of the Dimethyl Sulfide Complexes [OsX 4 (dms) 2 ] (Х = Cl, Br) and [Os 2 OCl 6 (dms) 4 ] Olga V. Rudnitskaya, Ekaterina V. Dobrokhotova, Tatiana A. Tereshina, and 6 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-8897604/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 14 You are reading this latest preprint version Abstract A systematic study of the thermal decomposition of osmium(IV) complexes [H(dmso) 2 ] 2 [OsX 6 ] and [H(dmso) 2 ][OsX 5 (dmso)] (dmso = dimethylsulfoxide; X = Cl, Br) was carried out. According to column chromatography (CC) data, the major thermolysis products in the temperature range of 100–140 ℃ (X = Cl) and 80–120 ℃ (X = Br) are the dimethyl sulfide (dms) osmium(IV) complexes trans- [OsX 4 (dms) 2 ] (X = Cl, Br) with yields of up to 85% (X = Cl) and 95% (X = Br). It also yielded a small amount of the dinuclear complex [Os 2 OCl 6 (dms) 4 ]. IR spectra of [OsX 4 (dms) 2 ] support the assumed trans conformation, 1 H NMR spectra show only one signal for the dms ligands. UV − Vis absorption spectra allowed to trace different species within distinct CC fractions, with the first fraction agreeing with the isolated crystalline material [OsX 4 (dms) 2 ]. The structures were determined by single crystal X-ray diffraction. The two polymorphic modifications were found for trans -[OsCl 4 (dms) 2 ]. The dinuclear [Os 2 OCl 6 (dms) 4 ] includes an oxide bridge between two trans -[OsCl 3 (dms) 2 ] fragments. Osmium complexes Dimethyl sulfide ligand Thermolysis Differential thermal analysis Spectrophotometry X-ray diffraction Full Text Additional Declarations No competing interests reported. Supplementary Files SCESIRudnitskaya2026.docx 5a.cif 5acheckcif.pdf 5b.cif 5bcheckcif.pdf 6.cif 6checkcif.pdf 7.cif 7checkcif.pdf Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 24 Mar, 2026 Reviews received at journal 23 Mar, 2026 Reviews received at journal 14 Mar, 2026 Reviews received at journal 28 Feb, 2026 Reviewers agreed at journal 28 Feb, 2026 Reviews received at journal 27 Feb, 2026 Reviewers agreed at journal 27 Feb, 2026 Reviewers agreed at journal 26 Feb, 2026 Reviewers agreed at journal 25 Feb, 2026 Reviewers agreed at journal 25 Feb, 2026 Reviewers invited by journal 24 Feb, 2026 Editor assigned by journal 24 Feb, 2026 Submission checks completed at journal 24 Feb, 2026 First submitted to journal 16 Feb, 2026 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-8897604","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":596910133,"identity":"3609a563-e1a1-4131-adb1-41b9e9429fc4","order_by":0,"name":"Olga V. 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]","fulltext":[],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":false,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":true,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":true,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"structural-chemistry","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"stuc","sideBox":"Learn more about [Structural Chemistry](https://www.springer.com/journal/11224)","snPcode":"11224","submissionUrl":"https://submission.nature.com/new-submission/11224/3","title":"Structural Chemistry","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Osmium complexes, Dimethyl sulfide ligand, Thermolysis, Differential thermal analysis, Spectrophotometry, X-ray diffraction","lastPublishedDoi":"10.21203/rs.3.rs-8897604/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-8897604/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eA systematic study of the thermal decomposition of osmium(IV) complexes [H(dmso)\u003csub\u003e2\u003c/sub\u003e]\u003csub\u003e2\u003c/sub\u003e[OsX\u003csub\u003e6\u003c/sub\u003e] and [H(dmso)\u003csub\u003e2\u003c/sub\u003e][OsX\u003csub\u003e5\u003c/sub\u003e(dmso)] (dmso\u0026thinsp;=\u0026thinsp;dimethylsulfoxide; X\u0026thinsp;=\u0026thinsp;Cl, Br) was carried out. According to column chromatography (CC) data, the major thermolysis products in the temperature range of 100\u0026ndash;140 ℃ (X\u0026thinsp;=\u0026thinsp;Cl) and 80\u0026ndash;120 ℃ (X\u0026thinsp;=\u0026thinsp;Br) are the dimethyl sulfide (dms) osmium(IV) complexes \u003cem\u003etrans-\u003c/em\u003e[OsX\u003csub\u003e4\u003c/sub\u003e(dms)\u003csub\u003e2\u003c/sub\u003e] (X\u0026thinsp;=\u0026thinsp;Cl, Br) with yields of up to 85% (X\u0026thinsp;=\u0026thinsp;Cl) and 95% (X\u0026thinsp;=\u0026thinsp;Br). It also yielded a small amount of the dinuclear complex [Os\u003csub\u003e2\u003c/sub\u003eOCl\u003csub\u003e6\u003c/sub\u003e(dms)\u003csub\u003e4\u003c/sub\u003e]. IR spectra of [OsX\u003csub\u003e4\u003c/sub\u003e(dms)\u003csub\u003e2\u003c/sub\u003e] support the assumed \u003cem\u003etrans\u003c/em\u003e conformation, \u003csup\u003e1\u003c/sup\u003eH NMR spectra show only one signal for the dms ligands. UV\u0026thinsp;\u0026minus;\u0026thinsp;Vis absorption spectra allowed to trace different species within distinct CC fractions, with the first fraction agreeing with the isolated crystalline material [OsX\u003csub\u003e4\u003c/sub\u003e(dms)\u003csub\u003e2\u003c/sub\u003e]. The structures were determined by single crystal X-ray diffraction. The two polymorphic modifications were found for \u003cem\u003etrans\u003c/em\u003e-[OsCl\u003csub\u003e4\u003c/sub\u003e(dms)\u003csub\u003e2\u003c/sub\u003e]. The dinuclear [Os\u003csub\u003e2\u003c/sub\u003eOCl\u003csub\u003e6\u003c/sub\u003e(dms)\u003csub\u003e4\u003c/sub\u003e] includes an oxide bridge between two \u003cem\u003etrans\u003c/em\u003e-[OsCl\u003csub\u003e3\u003c/sub\u003e(dms)\u003csub\u003e2\u003c/sub\u003e] fragments.\u003c/p\u003e","manuscriptTitle":"Synthesis and Structure of the Dimethyl Sulfide Complexes [OsX 4 (dms) 2 ] (Х = Cl, Br) and [Os 2 OCl 6 (dms) 4 ]","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2026-02-26 19:00:09","doi":"10.21203/rs.3.rs-8897604/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2026-03-24T13:20:17+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-03-23T06:46:09+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-03-14T16:15:40+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-02-28T18:44:31+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"28140910155219549660575288161356760177","date":"2026-02-28T10:21:46+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-02-27T11:22:18+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"165112526622686307297710481107538369038","date":"2026-02-27T09:12:57+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"253573666807798238206676770655946612646","date":"2026-02-26T09:32:17+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"160987351134435873832109052121377414294","date":"2026-02-25T11:55:40+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"60904890573043843484480657402529724033","date":"2026-02-25T08:26:59+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2026-02-24T14:27:31+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2026-02-24T13:39:22+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2026-02-24T12:49:15+00:00","index":"","fulltext":""},{"type":"submitted","content":"Structural Chemistry","date":"2026-02-17T04:56:56+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"structural-chemistry","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"stuc","sideBox":"Learn more about [Structural Chemistry](https://www.springer.com/journal/11224)","snPcode":"11224","submissionUrl":"https://submission.nature.com/new-submission/11224/3","title":"Structural Chemistry","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"a9692430-23e2-4810-bcd3-263be510365b","owner":[],"postedDate":"February 26th, 2026","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[],"tags":[],"updatedAt":"2026-04-20T13:25:51+00:00","versionOfRecord":[],"versionCreatedAt":"2026-02-26 19:00:09","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-8897604","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-8897604","identity":"rs-8897604","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}