Macrocycles containing 1,1′-ferrocenyldiselenolato ligands on group 4 metallocenes

Macrocyclic [Fe(η 5 -C 5 H 4 Se) 2 M(η 5 -C 5 H 4 R) 2 ] 2 [M = Ti ( 1 ), Zr ( 2 ), Hf ( 3 ), R = H; and M = Zr ( 4 ), Hf ( 5 ), R = t Bu] were prepared and characterized by 77 Se NMR spectroscopy and the crystal structures of 1-3 and 5 were determined by single-crystal X-ray diffraction. The crysta...

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Veröffentlicht in:Dalton transactions : an international journal of inorganic chemistry 2018-04, Vol.47 (15), p.5415-5421
Hauptverfasser: Sanchez-Perez, Clara, Knapp, Caroline E, Karjalainen, Minna M, Oilunkaniemi, Raija, Carmalt, Claire J, Laitinen, Risto S
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container_issue 15
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container_title Dalton transactions : an international journal of inorganic chemistry
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creator Sanchez-Perez, Clara
Knapp, Caroline E
Karjalainen, Minna M
Oilunkaniemi, Raija
Carmalt, Claire J
Laitinen, Risto S
description Macrocyclic [Fe(η 5 -C 5 H 4 Se) 2 M(η 5 -C 5 H 4 R) 2 ] 2 [M = Ti ( 1 ), Zr ( 2 ), Hf ( 3 ), R = H; and M = Zr ( 4 ), Hf ( 5 ), R = t Bu] were prepared and characterized by 77 Se NMR spectroscopy and the crystal structures of 1-3 and 5 were determined by single-crystal X-ray diffraction. The crystal structure of 4 is known and the complex is isomorphous with 5 . 1-5 form mutually similar macrocyclic tetranuclear complexes in which the alternating Fe(C 5 H 4 Se) 2 and M(C 5 H 4 R) 2 centers are linked by selenium bridges. The thermogravimetric analysis (TGA) of 1-3 under a helium atmosphere indicated that the complexes undergo a two-step decomposition upon heating. The final products were identified using powder X-ray diffraction as Fe x MSe 2 , indicating their potential as single-source precursors for functional materials. Macrocyclic [Fe(η 5 -C 5 H 4 Se) 2 M(η 5 -C 5 H 4 R) 2 ] 2 [M = Ti ( 1 ), Zr ( 2 ), Hf ( 3 ), R = H; and M = Zr ( 4 ), Hf ( 5 ), R = t Bu] were prepared and characterized by 77 Se NMR spectroscopy and the crystal structures of 1-3 and 5 were determined by single-crystal X-ray diffraction.
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The crystal structure of 4 is known and the complex is isomorphous with 5 . 1-5 form mutually similar macrocyclic tetranuclear complexes in which the alternating Fe(C 5 H 4 Se) 2 and M(C 5 H 4 R) 2 centers are linked by selenium bridges. The thermogravimetric analysis (TGA) of 1-3 under a helium atmosphere indicated that the complexes undergo a two-step decomposition upon heating. The final products were identified using powder X-ray diffraction as Fe x MSe 2 , indicating their potential as single-source precursors for functional materials. Macrocyclic [Fe(η 5 -C 5 H 4 Se) 2 M(η 5 -C 5 H 4 R) 2 ] 2 [M = Ti ( 1 ), Zr ( 2 ), Hf ( 3 ), R = H; and M = Zr ( 4 ), Hf ( 5 ), R = t Bu] were prepared and characterized by 77 Se NMR spectroscopy and the crystal structures of 1-3 and 5 were determined by single-crystal X-ray diffraction.</description><identifier>ISSN: 1477-9226</identifier><identifier>EISSN: 1477-9234</identifier><identifier>DOI: 10.1039/c8dt00300a</identifier><identifier>PMID: 29589863</identifier><language>eng</language><publisher>England: Royal Society of Chemistry</publisher><subject>Crystal structure ; Diffraction ; Hafnium ; Helium ; Metallocenes ; NMR spectroscopy ; Selenium ; Single crystals ; Thermogravimetric analysis ; Titanium ; X ray powder diffraction ; X-ray diffraction ; Zirconium</subject><ispartof>Dalton transactions : an international journal of inorganic chemistry, 2018-04, Vol.47 (15), p.5415-5421</ispartof><rights>Copyright Royal Society of Chemistry 2018</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c399t-a2825a87ddc35a5beb620ca21a859b99a80fe1817866630851dc17c25c9fda2b3</citedby><cites>FETCH-LOGICAL-c399t-a2825a87ddc35a5beb620ca21a859b99a80fe1817866630851dc17c25c9fda2b3</cites><orcidid>0000-0001-7070-8707 ; 0000-0003-1788-6971 ; 0000-0003-4219-9313</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,776,780,27901,27902</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/29589863$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Sanchez-Perez, Clara</creatorcontrib><creatorcontrib>Knapp, Caroline E</creatorcontrib><creatorcontrib>Karjalainen, Minna M</creatorcontrib><creatorcontrib>Oilunkaniemi, Raija</creatorcontrib><creatorcontrib>Carmalt, Claire J</creatorcontrib><creatorcontrib>Laitinen, Risto S</creatorcontrib><title>Macrocycles containing 1,1′-ferrocenyldiselenolato ligands on group 4 metallocenes</title><title>Dalton transactions : an international journal of inorganic chemistry</title><addtitle>Dalton Trans</addtitle><description>Macrocyclic [Fe(η 5 -C 5 H 4 Se) 2 M(η 5 -C 5 H 4 R) 2 ] 2 [M = Ti ( 1 ), Zr ( 2 ), Hf ( 3 ), R = H; and M = Zr ( 4 ), Hf ( 5 ), R = t Bu] were prepared and characterized by 77 Se NMR spectroscopy and the crystal structures of 1-3 and 5 were determined by single-crystal X-ray diffraction. 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source Royal Society Of Chemistry Journals 2008-; Alma/SFX Local Collection
subjects Crystal structure
Diffraction
Hafnium
Helium
Metallocenes
NMR spectroscopy
Selenium
Single crystals
Thermogravimetric analysis
Titanium
X ray powder diffraction
X-ray diffraction
Zirconium
title Macrocycles containing 1,1′-ferrocenyldiselenolato ligands on group 4 metallocenes
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