Heterometallic Ru-Ir hydride carbonyl clusters

Heterometallic Ru-Ir hydride carbonyl clusters | 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 Heterometallic Ru-Ir hydride carbonyl clusters Francesca Forti, Cristiana Cesari, Marco Bortoluzzi, Cristina Femoni, and 3 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-5025273/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 13 You are reading this latest preprint version Abstract [NEt 4 ][HRu 3 (CO) 11 ] ( 1 ) reacts with [Ir(COD)Cl] 2 in a 1 : 0.5 molar ratio under H 2 atmosphere affording the previously reported [NEt 4 ][H 2 Ru 3 Ir(CO) 12 ] ( 2 ). Performing the reaction under N 2 atmosphere with a 1 : 1 molar ratio of the reagents results in the new species [NEt 4 ][H 1–x Ru 3–x Ir 2+x (CO) 12 (COD)] (x = 0.11) ( 3 ), whereas H 2 − x Ru 3 − x Ir 2 + x (CO) 10 (COD) 2 (x = 0.5 and 0.77) ( 4 ) is obtained by further increasing the amount of [Ir(COD)Cl] 2 . In particular, compound 4 with x = 0.5 has been obtained with a 1 : 1.25 molar ratio of the reagents, whereas 4 with x = 0.77 is formed increasing the stoichiometry to 1 : 1.5. Reaction of 1 and [Ir(COD)Cl] 2 under CO atmosphere affords [NEt 4 ] 2 [Ru 4 Ir 2 (CO) 17 ] ( 5 ) (molar ratio of the reagents 1 : 0.7). Syntheses of 2–5 are very sensitive to the experimental conditions, and optimized procedures in order to obtain each of these compounds in good yield and high purity have been identified. Slight variations of the experimental conditions lead to lower yield and traces of side-products are formed, among which [NEt 4 ][H 2 Ru 3 Ir(CO) 10 (COD)] ( 6 ), [NEt 4 ][HRu 3 IrCl(CO) 12 ] ( 7 ), [NEt 4 ] 3 [HRu 2 Ir 2 (CO) 12 ]Cl 2 ( 8 ) and [NEt 4 ] 2 [Ru 4 (O)Cl 4 (CO) 10 ] ( 9 ) have been identified by single-crystal X-ray diffraction (SC-XRD). All the main products 2 – 5 have been structurally characterized by SC-XRD and further investigated by IR and 1 H NMR spectroscopy in solution. Hydride locations have been elucidated by computational methods. Heterometallic cluster Carbonyl ligand Ruthenium Iridium Hydride Full Text Additional Declarations No competing interests reported. Supplementary Files SI.docx Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 01 Oct, 2024 Reviews received at journal 01 Oct, 2024 Reviews received at journal 28 Sep, 2024 Reviews received at journal 27 Sep, 2024 Reviews received at journal 25 Sep, 2024 Reviewers agreed at journal 24 Sep, 2024 Reviewers agreed at journal 20 Sep, 2024 Reviewers agreed at journal 19 Sep, 2024 Reviewers agreed at journal 18 Sep, 2024 Reviewers invited by journal 18 Sep, 2024 Editor assigned by journal 06 Sep, 2024 Submission checks completed at journal 06 Sep, 2024 First submitted to journal 03 Sep, 2024 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. 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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-5025273","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":361239506,"identity":"44414807-029a-49c2-bc4e-2877cc582343","order_by":0,"name":"Francesca Forti","email":"","orcid":"","institution":"Università di Bologna","correspondingAuthor":false,"prefix":"","firstName":"Francesca","middleName":"","lastName":"Forti","suffix":""},{"id":361239507,"identity":"bb3c76a9-d3bf-432c-a843-b819b0a5b9e3","order_by":1,"name":"Cristiana 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clusters","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":"journal-of-cluster-science","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":" Learn more about [Journal of Cluster Science](https://www.springer.com/journal/10876) ","snPcode":"10876","submissionUrl":"https://mc.manuscriptcentral.com/jocl","title":"Journal of Cluster Science","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Heterometallic cluster, Carbonyl ligand, Ruthenium, Iridium, Hydride","lastPublishedDoi":"10.21203/rs.3.rs-5025273/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-5025273/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003e[NEt\u003csub\u003e4\u003c/sub\u003e][HRu\u003csub\u003e3\u003c/sub\u003e(CO)\u003csub\u003e11\u003c/sub\u003e] (\u003cb\u003e1\u003c/b\u003e) reacts with [Ir(COD)Cl]\u003csub\u003e2\u003c/sub\u003e in a 1 : 0.5 molar ratio under H\u003csub\u003e2\u003c/sub\u003e atmosphere affording the previously reported [NEt\u003csub\u003e4\u003c/sub\u003e][H\u003csub\u003e2\u003c/sub\u003eRu\u003csub\u003e3\u003c/sub\u003eIr(CO)\u003csub\u003e12\u003c/sub\u003e] (\u003cb\u003e2\u003c/b\u003e). Performing the reaction under N\u003csub\u003e2\u003c/sub\u003e atmosphere with a 1 : 1 molar ratio of the reagents results in the new species [NEt\u003csub\u003e4\u003c/sub\u003e][H\u003csub\u003e1\u0026ndash;x\u003c/sub\u003eRu\u003csub\u003e3\u0026ndash;x\u003c/sub\u003eIr\u003csub\u003e2+x\u003c/sub\u003e(CO)\u003csub\u003e12\u003c/sub\u003e(COD)] (x\u0026thinsp;=\u0026thinsp;0.11) (\u003cb\u003e3\u003c/b\u003e), whereas H\u003csub\u003e2\u0026thinsp;\u0026minus;\u0026thinsp;x\u003c/sub\u003eRu\u003csub\u003e3\u0026thinsp;\u0026minus;\u0026thinsp;x\u003c/sub\u003eIr\u003csub\u003e2\u0026thinsp;+\u0026thinsp;x\u003c/sub\u003e(CO)\u003csub\u003e10\u003c/sub\u003e(COD)\u003csub\u003e2\u003c/sub\u003e (x\u0026thinsp;=\u0026thinsp;0.5 and 0.77) (\u003cb\u003e4\u003c/b\u003e) is obtained by further increasing the amount of [Ir(COD)Cl]\u003csub\u003e2\u003c/sub\u003e. In particular, compound \u003cb\u003e4\u003c/b\u003e with x\u0026thinsp;=\u0026thinsp;0.5 has been obtained with a 1 : 1.25 molar ratio of the reagents, whereas \u003cb\u003e4\u003c/b\u003e with x\u0026thinsp;=\u0026thinsp;0.77 is formed increasing the stoichiometry to 1 : 1.5. Reaction of \u003cb\u003e1\u003c/b\u003e and [Ir(COD)Cl]\u003csub\u003e2\u003c/sub\u003e under CO atmosphere affords [NEt\u003csub\u003e4\u003c/sub\u003e]\u003csub\u003e2\u003c/sub\u003e[Ru\u003csub\u003e4\u003c/sub\u003eIr\u003csub\u003e2\u003c/sub\u003e(CO)\u003csub\u003e17\u003c/sub\u003e] (\u003cb\u003e5\u003c/b\u003e) (molar ratio of the reagents 1 : 0.7). Syntheses of \u003cb\u003e2\u0026ndash;5\u003c/b\u003e are very sensitive to the experimental conditions, and optimized procedures in order to obtain each of these compounds in good yield and high purity have been identified. Slight variations of the experimental conditions lead to lower yield and traces of side-products are formed, among which [NEt\u003csub\u003e4\u003c/sub\u003e][H\u003csub\u003e2\u003c/sub\u003eRu\u003csub\u003e3\u003c/sub\u003eIr(CO)\u003csub\u003e10\u003c/sub\u003e(COD)] (\u003cb\u003e6\u003c/b\u003e), [NEt\u003csub\u003e4\u003c/sub\u003e][HRu\u003csub\u003e3\u003c/sub\u003eIrCl(CO)\u003csub\u003e12\u003c/sub\u003e] (\u003cb\u003e7\u003c/b\u003e), [NEt\u003csub\u003e4\u003c/sub\u003e]\u003csub\u003e3\u003c/sub\u003e[HRu\u003csub\u003e2\u003c/sub\u003eIr\u003csub\u003e2\u003c/sub\u003e(CO)\u003csub\u003e12\u003c/sub\u003e]Cl\u003csub\u003e2\u003c/sub\u003e (\u003cb\u003e8\u003c/b\u003e) and [NEt\u003csub\u003e4\u003c/sub\u003e]\u003csub\u003e2\u003c/sub\u003e[Ru\u003csub\u003e4\u003c/sub\u003e(O)Cl\u003csub\u003e4\u003c/sub\u003e(CO)\u003csub\u003e10\u003c/sub\u003e] (\u003cb\u003e9\u003c/b\u003e) have been identified by single-crystal X-ray diffraction (SC-XRD). All the main products \u003cb\u003e2\u003c/b\u003e\u0026ndash;\u003cb\u003e5\u003c/b\u003e have been structurally characterized by SC-XRD and further investigated by IR and \u003csup\u003e1\u003c/sup\u003eH NMR spectroscopy in solution. Hydride locations have been elucidated by computational methods.\u003c/p\u003e","manuscriptTitle":"Heterometallic Ru-Ir hydride carbonyl clusters","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-10-10 08:49:34","doi":"10.21203/rs.3.rs-5025273/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2024-10-01T17:20:10+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-10-01T14:18:19+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-09-28T16:04:24+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-09-27T19:07:12+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-09-25T15:27:25+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"224637267198563544240715408079002339154","date":"2024-09-24T16:59:45+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"19826806668434768598598512635848726067","date":"2024-09-20T15:01:39+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"122538974041771093103565725475053169242","date":"2024-09-19T04:03:03+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"84877057103479956549494304388243331815","date":"2024-09-18T17:10:03+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-09-18T14:44:26+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2024-09-06T14:00:58+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2024-09-06T10:12:29+00:00","index":"","fulltext":""},{"type":"submitted","content":"Journal of Cluster Science","date":"2024-09-03T13:18:58+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"journal-of-cluster-science","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":" Learn more about [Journal of Cluster Science](https://www.springer.com/journal/10876) ","snPcode":"10876","submissionUrl":"https://mc.manuscriptcentral.com/jocl","title":"Journal of Cluster Science","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"4ee87d45-2d7c-43ad-b078-35f8cac0a9bd","owner":[],"postedDate":"October 10th, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[],"tags":[],"updatedAt":"2024-10-21T08:53:45+00:00","versionOfRecord":[],"versionCreatedAt":"2024-10-10 08:49:34","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-5025273","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-5025273","identity":"rs-5025273","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}