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

Identifieur interne : 001665 ( Istex/Checkpoint ); précédent : 001664; suivant : 001666

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

Auteurs : E. O. Schlemper [États-Unis]

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.

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DOI: 10.1007/BF01369834


Affiliations:


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ISTEX:88C777217DE22C59FB95823A8A86422CE05CD557

Le document en format XML

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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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