Synthesis of isotope enriched (CN3H6)2[57Fe(CN)5NO] starting from 57Fe

Christoph Janiak; Thomas Dorn; Hauke Paulsen; Bernd Wrackmeyer

doi:10.1002/1521-3749(200107)627:7<1663::AID-ZAAC1663>3.0.CO;2-#

Synthesis of isotope enriched (CN₃H₆)₂[⁵⁷Fe(CN)₅NO] starting from ⁵⁷Fe

Christoph Janiak^*, Thomas Dorn, Hauke Paulsen, Bernd Wrackmeyer

^*Korrespondierende/r Autor/-in für diese Arbeit

Institut für Physik

8 Zitate (Scopus)

Abstract

A high-yield, mmolar-scale synthesis of pure guanidinium nitroprusside, (CN₃H₆)₂[⁽⁵⁷⁾Fe(CN)₅NO] (GNP) from iron metal is described. The iron metal contained pieces of 95.3% ⁵⁷Fe together with normal iron so that an isotope enrichment in ⁵⁷Fe of 25% was achieved. Single-crystals of GNP could be grown in cubic shape and dimensions of about 3×4×4 mm³. The purity of the GNP product and the intermediates K₄[⁽⁵⁷⁾Fe(CN)₆] · 3 H₂O and Na₂[⁽⁵⁷⁾Fe-(CN)₅NO] · 2 H₂O was ascertained by ⁵⁷Fe Mössbauer spectroscopy as well as ¹³C, ¹⁴N and ⁵⁷Fe NMR spectroscopy. The ⁵⁷Fe NMR chemical shift for [⁽⁵⁷⁾Fe(CN)₅NO]^2- in GNP was detected at +2004.0 ppm [vs Fe(CO)₅].

Originalsprache	Englisch
Zeitschrift	Zeitschrift fur Anorganische und Allgemeine Chemie
Jahrgang	627
Ausgabenummer	7
Seiten (von - bis)	1663-1668
Seitenumfang	6
ISSN	0044-2313
DOIs	https://doi.org/10.1002/1521-3749(200107)627:7<1663::AID-ZAAC1663>3.0.CO;2-#
Publikationsstatus	Veröffentlicht - 01.01.2001

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10.1002/1521-3749(200107)627:7<1663::AID-ZAAC1663>3.0.CO;2-#

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@article{114511506221445594fab1ec6d67627e,

title = "Synthesis of isotope enriched (CN3H6)2[57Fe(CN)5NO] starting from 57Fe",

abstract = "A high-yield, mmolar-scale synthesis of pure guanidinium nitroprusside, (CN3H6)2[(57)Fe(CN)5NO] (GNP) from iron metal is described. The iron metal contained pieces of 95.3% 57Fe together with normal iron so that an isotope enrichment in 57Fe of 25% was achieved. Single-crystals of GNP could be grown in cubic shape and dimensions of about 3×4×4 mm3. The purity of the GNP product and the intermediates K4[(57)Fe(CN)6] · 3 H2O and Na2[(57)Fe-(CN)5NO] · 2 H2O was ascertained by 57Fe M{\"o}ssbauer spectroscopy as well as 13C, 14N and 57Fe NMR spectroscopy. The 57Fe NMR chemical shift for [(57)Fe(CN)5NO]2- in GNP was detected at +2004.0 ppm [vs Fe(CO)5].",

author = "Christoph Janiak and Thomas Dorn and Hauke Paulsen and Bernd Wrackmeyer",

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T1 - Synthesis of isotope enriched (CN3H6)2[57Fe(CN)5NO] starting from 57Fe

AU - Janiak, Christoph

AU - Dorn, Thomas

AU - Paulsen, Hauke

AU - Wrackmeyer, Bernd

PY - 2001/1/1

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N2 - A high-yield, mmolar-scale synthesis of pure guanidinium nitroprusside, (CN3H6)2[(57)Fe(CN)5NO] (GNP) from iron metal is described. The iron metal contained pieces of 95.3% 57Fe together with normal iron so that an isotope enrichment in 57Fe of 25% was achieved. Single-crystals of GNP could be grown in cubic shape and dimensions of about 3×4×4 mm3. The purity of the GNP product and the intermediates K4[(57)Fe(CN)6] · 3 H2O and Na2[(57)Fe-(CN)5NO] · 2 H2O was ascertained by 57Fe Mössbauer spectroscopy as well as 13C, 14N and 57Fe NMR spectroscopy. The 57Fe NMR chemical shift for [(57)Fe(CN)5NO]2- in GNP was detected at +2004.0 ppm [vs Fe(CO)5].

AB - A high-yield, mmolar-scale synthesis of pure guanidinium nitroprusside, (CN3H6)2[(57)Fe(CN)5NO] (GNP) from iron metal is described. The iron metal contained pieces of 95.3% 57Fe together with normal iron so that an isotope enrichment in 57Fe of 25% was achieved. Single-crystals of GNP could be grown in cubic shape and dimensions of about 3×4×4 mm3. The purity of the GNP product and the intermediates K4[(57)Fe(CN)6] · 3 H2O and Na2[(57)Fe-(CN)5NO] · 2 H2O was ascertained by 57Fe Mössbauer spectroscopy as well as 13C, 14N and 57Fe NMR spectroscopy. The 57Fe NMR chemical shift for [(57)Fe(CN)5NO]2- in GNP was detected at +2004.0 ppm [vs Fe(CO)5].

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