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Synthesis and X-ray diffraction study of hexaamminecobalt(III) sodium ethylenediaminetetraacetate 3.5-hydrate

Identifieur interne : 000D55 ( Istex/Corpus ); précédent : 000D54; suivant : 000D56

Synthesis and X-ray diffraction study of hexaamminecobalt(III) sodium ethylenediaminetetraacetate 3.5-hydrate

Auteurs : E. O. Schlemper

Source :

RBID : ISTEX:88C777217DE22C59FB95823A8A86422CE05CD557

English descriptors

Abstract

Abstract: The title compound [Co(NH3)6] [Na(EDTA-4H)],3.5H2O has been synthesized, and its crystal structure has been determined from 2064 independent single-crystal reflections measured on a diffractometer. The crystals are tetragonal, space groupP4212, with unit-cell parametersa = 14.618(5) andc = 10.658(4) Å. There are four formula entities in the unit cell givingD c = 1.562(2) g cm−3 compared withD m = 1.56(1) g cm−3. The structure was solved by conventional Patterson and Fourier techniques, and refined by full-matrix least-squares methods to a final agreement factor of 3.6%. The compound contains two crystallographically independent octahedral [Co(NH3)6]3+ ions, with an average Co—N distance of 1.966(6) Å, and a seven-coordinate sodium ion which is coordinated to four carboxyl oxygens, two amine nitrogens, and a water molecule which bridges to another sodium ion. The EDTA is therefore acting in its normal hexadentate manner. The range of Na—O distances is 2.25 to 2.93 Å whereas the Na—N distance is 2.46 Å. The crystal structure is additionally stabilized by extensive hydrogen bonding among coordinated ammonias, carboxyl oxygens, and water molecules.

Url:
DOI: 10.1007/BF01369834

Links to Exploration step

ISTEX:88C777217DE22C59FB95823A8A86422CE05CD557

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<div type="abstract" xml:lang="en">Abstract: The title compound [Co(NH3)6] [Na(EDTA-4H)],3.5H2O has been synthesized, and its crystal structure has been determined from 2064 independent single-crystal reflections measured on a diffractometer. The crystals are tetragonal, space groupP4212, with unit-cell parametersa = 14.618(5) andc = 10.658(4) Å. There are four formula entities in the unit cell givingD c = 1.562(2) g cm−3 compared withD m = 1.56(1) g cm−3. The structure was solved by conventional Patterson and Fourier techniques, and refined by full-matrix least-squares methods to a final agreement factor of 3.6%. The compound contains two crystallographically independent octahedral [Co(NH3)6]3+ ions, with an average Co—N distance of 1.966(6) Å, and a seven-coordinate sodium ion which is coordinated to four carboxyl oxygens, two amine nitrogens, and a water molecule which bridges to another sodium ion. The EDTA is therefore acting in its normal hexadentate manner. The range of Na—O distances is 2.25 to 2.93 Å whereas the Na—N distance is 2.46 Å. The crystal structure is additionally stabilized by extensive hydrogen bonding among coordinated ammonias, carboxyl oxygens, and water molecules.</div>
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<publisher>Kluwer Academic Publishers-Plenum Publishers</publisher>
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<dateCreated encoding="w3cdtf">1976-12-24</dateCreated>
<dateIssued encoding="w3cdtf">1977-04-01</dateIssued>
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<abstract lang="en">Abstract: The title compound [Co(NH3)6] [Na(EDTA-4H)],3.5H2O has been synthesized, and its crystal structure has been determined from 2064 independent single-crystal reflections measured on a diffractometer. The crystals are tetragonal, space groupP4212, with unit-cell parametersa = 14.618(5) andc = 10.658(4) Å. There are four formula entities in the unit cell givingD c = 1.562(2) g cm−3 compared withD m = 1.56(1) g cm−3. The structure was solved by conventional Patterson and Fourier techniques, and refined by full-matrix least-squares methods to a final agreement factor of 3.6%. The compound contains two crystallographically independent octahedral [Co(NH3)6]3+ ions, with an average Co—N distance of 1.966(6) Å, and a seven-coordinate sodium ion which is coordinated to four carboxyl oxygens, two amine nitrogens, and a water molecule which bridges to another sodium ion. The EDTA is therefore acting in its normal hexadentate manner. The range of Na—O distances is 2.25 to 2.93 Å whereas the Na—N distance is 2.46 Å. The crystal structure is additionally stabilized by extensive hydrogen bonding among coordinated ammonias, carboxyl oxygens, and water molecules.</abstract>
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<title>Journal of Crystal and Molecular Structure</title>
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<titleInfo type="abbreviated">
<title>Journal of Crystal and Molecular Structure</title>
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<publisher>Springer</publisher>
<dateIssued encoding="w3cdtf">1977-04-01</dateIssued>
<copyrightDate encoding="w3cdtf">1977</copyrightDate>
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<subject>
<genre>Chemistry</genre>
<topic>Inorganic Chemistry</topic>
<topic>Organometallic Chemistry</topic>
<topic>Physical Chemistry</topic>
<topic>Crystallography</topic>
</subject>
<identifier type="ISSN">0308-4086</identifier>
<identifier type="eISSN">1572-8854</identifier>
<identifier type="JournalID">10870</identifier>
<identifier type="IssueArticleCount">4</identifier>
<identifier type="VolumeIssueCount">6</identifier>
<part>
<date>1977</date>
<detail type="volume">
<number>7</number>
<caption>vol.</caption>
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<detail type="issue">
<number>2</number>
<caption>no.</caption>
</detail>
<extent unit="pages">
<start>81</start>
<end>93</end>
</extent>
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<recordOrigin>Plenum Publishing Corporation, 1977</recordOrigin>
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<identifier type="istex">88C777217DE22C59FB95823A8A86422CE05CD557</identifier>
<identifier type="ark">ark:/67375/1BB-12FMVJGD-D</identifier>
<identifier type="DOI">10.1007/BF01369834</identifier>
<identifier type="ArticleID">BF01369834</identifier>
<identifier type="ArticleID">Art3</identifier>
<accessCondition type="use and reproduction" contentType="copyright">Plenum Publishing Corporation, 1977</accessCondition>
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<recordOrigin>Plenum Publishing Corporation, 1977</recordOrigin>
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