Selective P 4 Activation by a Highly Reduced Cobaltate: Synthesis of Dicobalt Tetraphosphido Complexes
Although the chemistry of transition metal polyphosphide anions has attracted significant attention, there are few reports of studies in which such species have been synthesized directly from white phosphorus. [K(OEt ) {Co(BIAN)(cod)}] (1, BIAN=1,2-bis(2,6-diisopropylphenylimino)acenaphthene, cod=1,...
Gespeichert in:
Veröffentlicht in: | Chemistry : a European journal 2017-05, Vol.23 (25), p.6094-6102 |
---|---|
Hauptverfasser: | , , , , , , , |
Format: | Artikel |
Sprache: | eng |
Online-Zugang: | Volltext |
Tags: |
Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
|
container_end_page | 6102 |
---|---|
container_issue | 25 |
container_start_page | 6094 |
container_title | Chemistry : a European journal |
container_volume | 23 |
creator | Pelties, Stefan Maier, Thomas Herrmann, Dirk de Bruin, Bas Rebreyend, Christophe Gärtner, Stefanie Shenderovich, Ilya G Wolf, Robert |
description | Although the chemistry of transition metal polyphosphide anions has attracted significant attention, there are few reports of studies in which such species have been synthesized directly from white phosphorus. [K(OEt
)
{Co(BIAN)(cod)}] (1, BIAN=1,2-bis(2,6-diisopropylphenylimino)acenaphthene, cod=1,5-cyclooctadiene), which is readily prepared by ligand exchange from [K(thf)
{Co(cod)
}], reacts with P
to afford [{K(thf)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 a) in 61 % yield (isolated product). [{K(OEt
)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 b) and [K([18]crown-6)(MeCN)]
[{(BIAN)Co}
(μ-η
:η
-P
)] (2 c) were obtained by recrystallizing 2 a from diethyl ether and acetonitrile (and using [18]crown-6 in case of 2 c). Oxidation of 2 a with [Cp
Fe]BAr
(one equivalent) and subsequent recrystallization of the product from different solvents gave [K(OEt
){(BIAN)Co}
(μ-η
:η
-P
)] (3 a) and [K(dme)
][{(BIAN)Co}
(μ-η
:η
-P
)] (3 b; dme=1,2-dimethoxyethane). Neutral [{(BIAN)Co}
(μ-η
:η
-P
)] (4) was obtained in moderate yield by oxidizing 2 a with two equivalents of [Cp
Fe]BAr
. The new complexes were characterized by NMR, EPR (in the case of 3 a), and UV/Vis spectroscopy, and elemental analysis. The molecular structures revealed by X-ray crystallography display planar cyclic or open-chain P
units sandwiched between {(BIAN)Co} fragments. |
doi_str_mv | 10.1002/chem.201603296 |
format | Article |
fullrecord | <record><control><sourceid>pubmed_cross</sourceid><recordid>TN_cdi_crossref_primary_10_1002_chem_201603296</recordid><sourceformat>XML</sourceformat><sourcesystem>PC</sourcesystem><sourcerecordid>27651298</sourcerecordid><originalsourceid>FETCH-LOGICAL-c192t-fb609b925d20f0345f12e21e5b98ce2f0080b771abc52b7f9090db42cf39916d3</originalsourceid><addsrcrecordid>eNo9kMtOwzAURC0EoqWwZYn8AwnXduzU7KryKFIlEC3ryHauSVDSRHGKyN_TUuhqRprH4hByzSBmAPzWFVjHHJgCwbU6IWMmOYtEquQpGYNO0khJoUfkIoRPANBKiHMy4ruccT0dE7_CCl1ffiF9pQmd7a3py2ZD7UANXZQfRTXQN8y3DnM6b6ypetPjHV0Nm77AUAbaeHpfut-ErrHvTFs0oS3KvNn167bCbwyX5MybKuDVn07I--PDer6Ili9Pz_PZMnJM8z7yVoG2msucgweRSM84cobS6qlD7gGmYNOUGeskt6nXoCG3CXdeaM1ULiYkPvy6rgmhQ5-1XVmbbsgYZHtg2R5YdgS2G9wcBu3W1pgf6_-ExA9sC2c-</addsrcrecordid><sourcetype>Aggregation Database</sourcetype><iscdi>true</iscdi><recordtype>article</recordtype></control><display><type>article</type><title>Selective P 4 Activation by a Highly Reduced Cobaltate: Synthesis of Dicobalt Tetraphosphido Complexes</title><source>Access via Wiley Online Library</source><creator>Pelties, Stefan ; Maier, Thomas ; Herrmann, Dirk ; de Bruin, Bas ; Rebreyend, Christophe ; Gärtner, Stefanie ; Shenderovich, Ilya G ; Wolf, Robert</creator><creatorcontrib>Pelties, Stefan ; Maier, Thomas ; Herrmann, Dirk ; de Bruin, Bas ; Rebreyend, Christophe ; Gärtner, Stefanie ; Shenderovich, Ilya G ; Wolf, Robert</creatorcontrib><description>Although the chemistry of transition metal polyphosphide anions has attracted significant attention, there are few reports of studies in which such species have been synthesized directly from white phosphorus. [K(OEt
)
{Co(BIAN)(cod)}] (1, BIAN=1,2-bis(2,6-diisopropylphenylimino)acenaphthene, cod=1,5-cyclooctadiene), which is readily prepared by ligand exchange from [K(thf)
{Co(cod)
}], reacts with P
to afford [{K(thf)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 a) in 61 % yield (isolated product). [{K(OEt
)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 b) and [K([18]crown-6)(MeCN)]
[{(BIAN)Co}
(μ-η
:η
-P
)] (2 c) were obtained by recrystallizing 2 a from diethyl ether and acetonitrile (and using [18]crown-6 in case of 2 c). Oxidation of 2 a with [Cp
Fe]BAr
(one equivalent) and subsequent recrystallization of the product from different solvents gave [K(OEt
){(BIAN)Co}
(μ-η
:η
-P
)] (3 a) and [K(dme)
][{(BIAN)Co}
(μ-η
:η
-P
)] (3 b; dme=1,2-dimethoxyethane). Neutral [{(BIAN)Co}
(μ-η
:η
-P
)] (4) was obtained in moderate yield by oxidizing 2 a with two equivalents of [Cp
Fe]BAr
. The new complexes were characterized by NMR, EPR (in the case of 3 a), and UV/Vis spectroscopy, and elemental analysis. The molecular structures revealed by X-ray crystallography display planar cyclic or open-chain P
units sandwiched between {(BIAN)Co} fragments.</description><identifier>ISSN: 0947-6539</identifier><identifier>EISSN: 1521-3765</identifier><identifier>DOI: 10.1002/chem.201603296</identifier><identifier>PMID: 27651298</identifier><language>eng</language><publisher>Germany</publisher><ispartof>Chemistry : a European journal, 2017-05, Vol.23 (25), p.6094-6102</ispartof><rights>2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c192t-fb609b925d20f0345f12e21e5b98ce2f0080b771abc52b7f9090db42cf39916d3</citedby><cites>FETCH-LOGICAL-c192t-fb609b925d20f0345f12e21e5b98ce2f0080b771abc52b7f9090db42cf39916d3</cites><orcidid>0000-0001-6713-9080 ; 0000-0003-4066-6483</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>315,782,786,27931,27932</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/27651298$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Pelties, Stefan</creatorcontrib><creatorcontrib>Maier, Thomas</creatorcontrib><creatorcontrib>Herrmann, Dirk</creatorcontrib><creatorcontrib>de Bruin, Bas</creatorcontrib><creatorcontrib>Rebreyend, Christophe</creatorcontrib><creatorcontrib>Gärtner, Stefanie</creatorcontrib><creatorcontrib>Shenderovich, Ilya G</creatorcontrib><creatorcontrib>Wolf, Robert</creatorcontrib><title>Selective P 4 Activation by a Highly Reduced Cobaltate: Synthesis of Dicobalt Tetraphosphido Complexes</title><title>Chemistry : a European journal</title><addtitle>Chemistry</addtitle><description>Although the chemistry of transition metal polyphosphide anions has attracted significant attention, there are few reports of studies in which such species have been synthesized directly from white phosphorus. [K(OEt
)
{Co(BIAN)(cod)}] (1, BIAN=1,2-bis(2,6-diisopropylphenylimino)acenaphthene, cod=1,5-cyclooctadiene), which is readily prepared by ligand exchange from [K(thf)
{Co(cod)
}], reacts with P
to afford [{K(thf)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 a) in 61 % yield (isolated product). [{K(OEt
)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 b) and [K([18]crown-6)(MeCN)]
[{(BIAN)Co}
(μ-η
:η
-P
)] (2 c) were obtained by recrystallizing 2 a from diethyl ether and acetonitrile (and using [18]crown-6 in case of 2 c). Oxidation of 2 a with [Cp
Fe]BAr
(one equivalent) and subsequent recrystallization of the product from different solvents gave [K(OEt
){(BIAN)Co}
(μ-η
:η
-P
)] (3 a) and [K(dme)
][{(BIAN)Co}
(μ-η
:η
-P
)] (3 b; dme=1,2-dimethoxyethane). Neutral [{(BIAN)Co}
(μ-η
:η
-P
)] (4) was obtained in moderate yield by oxidizing 2 a with two equivalents of [Cp
Fe]BAr
. The new complexes were characterized by NMR, EPR (in the case of 3 a), and UV/Vis spectroscopy, and elemental analysis. The molecular structures revealed by X-ray crystallography display planar cyclic or open-chain P
units sandwiched between {(BIAN)Co} fragments.</description><issn>0947-6539</issn><issn>1521-3765</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2017</creationdate><recordtype>article</recordtype><recordid>eNo9kMtOwzAURC0EoqWwZYn8AwnXduzU7KryKFIlEC3ryHauSVDSRHGKyN_TUuhqRprH4hByzSBmAPzWFVjHHJgCwbU6IWMmOYtEquQpGYNO0khJoUfkIoRPANBKiHMy4ruccT0dE7_CCl1ffiF9pQmd7a3py2ZD7UANXZQfRTXQN8y3DnM6b6ypetPjHV0Nm77AUAbaeHpfut-ErrHvTFs0oS3KvNn167bCbwyX5MybKuDVn07I--PDer6Ili9Pz_PZMnJM8z7yVoG2msucgweRSM84cobS6qlD7gGmYNOUGeskt6nXoCG3CXdeaM1ULiYkPvy6rgmhQ5-1XVmbbsgYZHtg2R5YdgS2G9wcBu3W1pgf6_-ExA9sC2c-</recordid><startdate>20170502</startdate><enddate>20170502</enddate><creator>Pelties, Stefan</creator><creator>Maier, Thomas</creator><creator>Herrmann, Dirk</creator><creator>de Bruin, Bas</creator><creator>Rebreyend, Christophe</creator><creator>Gärtner, Stefanie</creator><creator>Shenderovich, Ilya G</creator><creator>Wolf, Robert</creator><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><orcidid>https://orcid.org/0000-0001-6713-9080</orcidid><orcidid>https://orcid.org/0000-0003-4066-6483</orcidid></search><sort><creationdate>20170502</creationdate><title>Selective P 4 Activation by a Highly Reduced Cobaltate: Synthesis of Dicobalt Tetraphosphido Complexes</title><author>Pelties, Stefan ; Maier, Thomas ; Herrmann, Dirk ; de Bruin, Bas ; Rebreyend, Christophe ; Gärtner, Stefanie ; Shenderovich, Ilya G ; Wolf, Robert</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c192t-fb609b925d20f0345f12e21e5b98ce2f0080b771abc52b7f9090db42cf39916d3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2017</creationdate><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Pelties, Stefan</creatorcontrib><creatorcontrib>Maier, Thomas</creatorcontrib><creatorcontrib>Herrmann, Dirk</creatorcontrib><creatorcontrib>de Bruin, Bas</creatorcontrib><creatorcontrib>Rebreyend, Christophe</creatorcontrib><creatorcontrib>Gärtner, Stefanie</creatorcontrib><creatorcontrib>Shenderovich, Ilya G</creatorcontrib><creatorcontrib>Wolf, Robert</creatorcontrib><collection>PubMed</collection><collection>CrossRef</collection><jtitle>Chemistry : a European journal</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Pelties, Stefan</au><au>Maier, Thomas</au><au>Herrmann, Dirk</au><au>de Bruin, Bas</au><au>Rebreyend, Christophe</au><au>Gärtner, Stefanie</au><au>Shenderovich, Ilya G</au><au>Wolf, Robert</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Selective P 4 Activation by a Highly Reduced Cobaltate: Synthesis of Dicobalt Tetraphosphido Complexes</atitle><jtitle>Chemistry : a European journal</jtitle><addtitle>Chemistry</addtitle><date>2017-05-02</date><risdate>2017</risdate><volume>23</volume><issue>25</issue><spage>6094</spage><epage>6102</epage><pages>6094-6102</pages><issn>0947-6539</issn><eissn>1521-3765</eissn><abstract>Although the chemistry of transition metal polyphosphide anions has attracted significant attention, there are few reports of studies in which such species have been synthesized directly from white phosphorus. [K(OEt
)
{Co(BIAN)(cod)}] (1, BIAN=1,2-bis(2,6-diisopropylphenylimino)acenaphthene, cod=1,5-cyclooctadiene), which is readily prepared by ligand exchange from [K(thf)
{Co(cod)
}], reacts with P
to afford [{K(thf)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 a) in 61 % yield (isolated product). [{K(OEt
)}
{(BIAN)Co}
(μ-η
:η
-P
)] (2 b) and [K([18]crown-6)(MeCN)]
[{(BIAN)Co}
(μ-η
:η
-P
)] (2 c) were obtained by recrystallizing 2 a from diethyl ether and acetonitrile (and using [18]crown-6 in case of 2 c). Oxidation of 2 a with [Cp
Fe]BAr
(one equivalent) and subsequent recrystallization of the product from different solvents gave [K(OEt
){(BIAN)Co}
(μ-η
:η
-P
)] (3 a) and [K(dme)
][{(BIAN)Co}
(μ-η
:η
-P
)] (3 b; dme=1,2-dimethoxyethane). Neutral [{(BIAN)Co}
(μ-η
:η
-P
)] (4) was obtained in moderate yield by oxidizing 2 a with two equivalents of [Cp
Fe]BAr
. The new complexes were characterized by NMR, EPR (in the case of 3 a), and UV/Vis spectroscopy, and elemental analysis. The molecular structures revealed by X-ray crystallography display planar cyclic or open-chain P
units sandwiched between {(BIAN)Co} fragments.</abstract><cop>Germany</cop><pmid>27651298</pmid><doi>10.1002/chem.201603296</doi><tpages>9</tpages><orcidid>https://orcid.org/0000-0001-6713-9080</orcidid><orcidid>https://orcid.org/0000-0003-4066-6483</orcidid></addata></record> |
fulltext | fulltext |
identifier | ISSN: 0947-6539 |
ispartof | Chemistry : a European journal, 2017-05, Vol.23 (25), p.6094-6102 |
issn | 0947-6539 1521-3765 |
language | eng |
recordid | cdi_crossref_primary_10_1002_chem_201603296 |
source | Access via Wiley Online Library |
title | Selective P 4 Activation by a Highly Reduced Cobaltate: Synthesis of Dicobalt Tetraphosphido Complexes |
url | https://sfx.bib-bvb.de/sfx_tum?ctx_ver=Z39.88-2004&ctx_enc=info:ofi/enc:UTF-8&ctx_tim=2024-12-05T18%3A55%3A50IST&url_ver=Z39.88-2004&url_ctx_fmt=infofi/fmt:kev:mtx:ctx&rfr_id=info:sid/primo.exlibrisgroup.com:primo3-Article-pubmed_cross&rft_val_fmt=info:ofi/fmt:kev:mtx:journal&rft.genre=article&rft.atitle=Selective%20P%204%20Activation%20by%20a%20Highly%20Reduced%20Cobaltate:%20Synthesis%20of%20Dicobalt%20Tetraphosphido%20Complexes&rft.jtitle=Chemistry%20:%20a%20European%20journal&rft.au=Pelties,%20Stefan&rft.date=2017-05-02&rft.volume=23&rft.issue=25&rft.spage=6094&rft.epage=6102&rft.pages=6094-6102&rft.issn=0947-6539&rft.eissn=1521-3765&rft_id=info:doi/10.1002/chem.201603296&rft_dat=%3Cpubmed_cross%3E27651298%3C/pubmed_cross%3E%3Curl%3E%3C/url%3E&disable_directlink=true&sfx.directlink=off&sfx.report_link=0&rft_id=info:oai/&rft_id=info:pmid/27651298&rfr_iscdi=true |