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Synthese, Charakterisierung und Kristallstrukturen der Pseudohalogen-Kronenether-Komplexe [K([18]krone-6)(X)(OPPh3)] (X = N3–, OCN– und SCN–)

2001; Wiley; Volume: 627; Issue: 11 Linguagem: Inglês

10.1002/1521-3749(200111)627

1521-3749

E. Kessenich, Κ. Polborn, Axel Schulz,

Magnetism in coordination complexes

Die Kaliumkronenetherkomplexe [K([18]krone-6)(X)(OPPh3)], mit X = N3–, OCN–, und SCN–, werden durch Reaktion von KX mit [18]Krone-6 (1, 4, 7, 10, 13, 16-Hexaoxacyclooctadekan) und Triphenylphosphan in mit UV Licht bestrahltem THF erhalten. Alle drei Kronenetherkomplexe konnten mit Hilfe der Schwingungsspektroskopie und der Röntgenstrukturanalyse charakterisiert werden. Die Kronenetherkomplexe kristallisieren isotyp in der rhombischen Raumgruppe R3m mit drei Molekülen in der Elementarzelle: [K([18]krone-6)(N3)(OPPh3)] (1): Gitterkonstanten bei 293 K: a = b = 14.213(2) Å; c = 13.951(2) Å; R1 = 0.0249. [K([18]krone-6)(OCN)(OPPh3)] (2): a = b = 14.239(2) Å; c = 13.8927(14) Å; R1 = 0.0257. [K([18]krone-6)(NCS)(OPPh3)] (3): a = b = 14.339(2) Å; c = 14.266(2) Å; R1 = 0.0264. Preparation, Characterisation, and Crystal Structures of the Pseudohalogen Crown Ether Complexes [K([18]crown-6)(X)(OPPh3)] (X = N3–, OCN– and SCN–) The potassium crown ether complexes [K([18]Crown-6)(X)(OPPh3)] (with X = N3–, OCN– and SCN–) can be obtained by reaction of KX with 18-crown-6 (1, 4, 7, 10, 13, 16-hexaoxacyclooctadecane and triphenylphosphane in THF exposed to UV light. All crown ether complexes were characterized by means of vibrational spectroscopy and X-ray diffraction. They crystallize in the rhombic pointgroup R3m with three molecules in the unit cell: [K([18]crown-6) (N3)(OPPh3)] (1): lattice constants at 293 K: a = b = 14.213(2) Å; c = 13.951(2) Å; R1 = 0.0249. [K([18]crown-6)(OCN)(OPPh3)] (2): a = b = 14.239(2) Å; c = 13.8927(14) Å; R1 = 0.0257. [K([18]crown-6)(NCS)(OPPh3)] (3): a = b = 14.339(2) Å; c = 14.266(2) Å; R1 = 0.0264.