Über Molekular‐ und Atomvolumina. X. Volumina einiger komplexer Kobaltsalze

Birk, Erwin; Biltz, Wilhelm

doi:10.1002/zaac.19261530112

Cited by 22 publications

(1 citation statement)

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“…Compound 6 was prepared by published methods [6] and single crystals suitable for Xray crystallographic studies were grown from a hot aqueous solution containing ammonium oxalate (to increase the solubility) [7] by slow cooling in a Dewar flask. Compound 6 was prepared by published methods [6] and single crystals suitable for Xray crystallographic studies were grown from a hot aqueous solution containing ammonium oxalate (to increase the solubility) [7] by slow cooling in a Dewar flask.…”

Section: Introductionmentioning

confidence: 99%

Untitled

Gorol

Mösch‐Zanetti

Noltemeyer

et al. 2000

Z. anorg. allg. Chem.

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Reaction of [M(NH 3 ) 6 ]Cl 3 (M = Co, Rh, Ir) and [Ir(NH 3 ) 5 (OH 2 )]Cl 3 with (NH 4 ) 2 C 2 O 4´H2 O in aqueous solution resulted in the isolation of [M(NH 3 ) 6 ] 2 (C 2 O 4 ) 3´4 H 2 O and [Ir(NH 3 ) 5 (OH 2 )] 2 (C 2 O 4 ) 3´4 H 2 O, respectively. The complexes have been characterized by X-ray crystallography, IR and UV/VIS spectroscopy. The isomorphous compounds crystallize in the orthorhombic space group Pnnm (No. 58). Four molecules of crystal water are involved in an extended three-dimensional hydrogen bonding network. The librational modes of the lattice water around 600 cm ±1 allow the characterization of [Ir(NH 3 ) 6 ] 2 (C 2 O 4 ) 3´4 H 2 O and [Ir(NH 3 ) 5 (OH 2 )] 2 (C 2 O 4 ) 3´4 H 2 O, respectively, by IR spectroscopy. The band around 600 cm ±1 shows a significant frequency shift in the IR spectra of the hexaammine and aquapentaammine complex of iridium(III) and, by that, a distinction is possible. Wasserlo È sliche und halogenfreie Hexaamminkomplexe von Metallionen der 9. Gruppe ± Darstellung, Kristallstrukturen und Schwingungsspektren Inhaltsu È bersicht. Die halogenfreien und wasserlo È slichen Verbindungen [M(NH 3 ) 6 ] 2 (C 2 O 4 ) 3´4 H 2 O und [Ir(NH 3 ) 5 -(OH 2 )] 2 (C 2 O 4 ) 3´4 H 2 O (M = Co, Rh, Ir) konnten durch Umsetzung von [M(NH 3 ) 6 ]Cl 3 und [Ir(NH 3 ) 5 (OH 2 )]Cl 3 mit (NH 4 ) 2 C 2 O 4´H2 O in wa È ssriger Lo È sung dargestellt werden. Die Komplexe wurden durch Einkristallstrukturanalyse, IR und UV/VIS Spektroskopie charakterisiert. Die isomorphen Verbindungen kristallisieren orthorhombisch in der Raumgruppe Pnnm (No. 58). Die vier Kristallwassermoleku È le sind an einem dreidimensionalen Netzwerk von Wasserstoffbru È kkenbindungen beteiligt. Die Librationen dieser Kristallwassermoleku È le liegen etwa bei 600 cm ±1 und ermo È glichen die Charakterisierung von [Ir(NH 3 ) 6 ] 2 (C 2 O 4 ) 3´4 H 2 O und [Ir(NH 3 ) 5 (OH 2 )] 2 (C 2 O 4 ) 3´4 H 2 O durch IR Spektroskopie. Diese Bande bei etwa 600 cm ±1 zeigt eine deutliche Verschiebung in den IR Spektren des Hexaamminiridium(III) und des Aquapentaamminiridium(III) Komplexes und ermo È glicht somit deren Unterscheidung.

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