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 |
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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. |
doi_str_mv | 10.1039/c8dt00300a |
format | Article |
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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.</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. 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><subject>Crystal structure</subject><subject>Diffraction</subject><subject>Hafnium</subject><subject>Helium</subject><subject>Metallocenes</subject><subject>NMR spectroscopy</subject><subject>Selenium</subject><subject>Single crystals</subject><subject>Thermogravimetric analysis</subject><subject>Titanium</subject><subject>X ray powder diffraction</subject><subject>X-ray diffraction</subject><subject>Zirconium</subject><issn>1477-9226</issn><issn>1477-9234</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2018</creationdate><recordtype>article</recordtype><recordid>eNp9kbtOwzAUhi0EoqWwsIOCWBAi4Euc2GNVrlIRS5kjx3aqVK5d7GToxjPxSDwJLi1FYmA6R_o__Tr6DgDHCF4jSPiNZKqFkEAodkAfZUWRckyy3e2O8x44CGEGIcaQ4n3Qw5wyznLSB5NnIb2TS2l0SKSzrWhsY6cJukKf7x9prX1MtV0a1QRttHVGtC4xzVRYFRJnk6l33SLJkrluhTErVodDsFcLE_TRZg7A6_3dZPSYjl8enkbDcSoJ520qMMNUsEIpSaigla5yDKXASDDKK84Fg7VGDBUsz3MCGUVKokJiKnmtBK7IAFysexfevXU6tOW8CVIbI6x2XSgxRDwrMIo6BuD8DzpznbfxukhhygtOMI_U5ZqKTkLwui4XvpkLvywRLFeuyxG7nXy7Hkb4dFPZVXOttuiP3AicrAEf5Db9fVbMz_7Ly4WqyRf0448p</recordid><startdate>20180417</startdate><enddate>20180417</enddate><creator>Sanchez-Perez, Clara</creator><creator>Knapp, Caroline E</creator><creator>Karjalainen, Minna M</creator><creator>Oilunkaniemi, Raija</creator><creator>Carmalt, Claire J</creator><creator>Laitinen, Risto S</creator><general>Royal Society of Chemistry</general><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope><scope>7X8</scope><orcidid>https://orcid.org/0000-0001-7070-8707</orcidid><orcidid>https://orcid.org/0000-0003-1788-6971</orcidid><orcidid>https://orcid.org/0000-0003-4219-9313</orcidid></search><sort><creationdate>20180417</creationdate><title>Macrocycles containing 1,1′-ferrocenyldiselenolato ligands on group 4 metallocenes</title><author>Sanchez-Perez, Clara ; Knapp, Caroline E ; Karjalainen, Minna M ; Oilunkaniemi, Raija ; Carmalt, Claire J ; Laitinen, Risto S</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c399t-a2825a87ddc35a5beb620ca21a859b99a80fe1817866630851dc17c25c9fda2b3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2018</creationdate><topic>Crystal structure</topic><topic>Diffraction</topic><topic>Hafnium</topic><topic>Helium</topic><topic>Metallocenes</topic><topic>NMR spectroscopy</topic><topic>Selenium</topic><topic>Single crystals</topic><topic>Thermogravimetric analysis</topic><topic>Titanium</topic><topic>X ray powder diffraction</topic><topic>X-ray diffraction</topic><topic>Zirconium</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><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><collection>PubMed</collection><collection>CrossRef</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>MEDLINE - Academic</collection><jtitle>Dalton transactions : an international journal of inorganic chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Sanchez-Perez, Clara</au><au>Knapp, Caroline E</au><au>Karjalainen, Minna M</au><au>Oilunkaniemi, Raija</au><au>Carmalt, Claire J</au><au>Laitinen, Risto S</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Macrocycles containing 1,1′-ferrocenyldiselenolato ligands on group 4 metallocenes</atitle><jtitle>Dalton transactions : an international journal of inorganic chemistry</jtitle><addtitle>Dalton Trans</addtitle><date>2018-04-17</date><risdate>2018</risdate><volume>47</volume><issue>15</issue><spage>5415</spage><epage>5421</epage><pages>5415-5421</pages><issn>1477-9226</issn><eissn>1477-9234</eissn><abstract>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.</abstract><cop>England</cop><pub>Royal Society of Chemistry</pub><pmid>29589863</pmid><doi>10.1039/c8dt00300a</doi><tpages>7</tpages><orcidid>https://orcid.org/0000-0001-7070-8707</orcidid><orcidid>https://orcid.org/0000-0003-1788-6971</orcidid><orcidid>https://orcid.org/0000-0003-4219-9313</orcidid><oa>free_for_read</oa></addata></record> |
fulltext | fulltext |
identifier | ISSN: 1477-9226 |
ispartof | Dalton transactions : an international journal of inorganic chemistry, 2018-04, Vol.47 (15), p.5415-5421 |
issn | 1477-9226 1477-9234 |
language | eng |
recordid | cdi_crossref_primary_10_1039_C8DT00300A |
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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